TY - JOUR A1 - Arinchtein, A. A1 - Ye, M.-Y. A1 - Yang, Q. A1 - Kreyenschulte, C. A1 - Wagner, Andreas A1 - Frisch, M. A1 - Brückner, A. A1 - Kondratenko, E. A1 - Kraehnert, R. T1 - Dynamics of Reaction-Induced Changes of Model-Type Iron Oxide Phases in the CO2-Fischer-Tropsch-Synthesis N2 - Iron-based catalysts are employed in CO2-FTS due to their ability to convert CO2 into CO in a first step and their selectivity towards higher hydrocarbons in a second CO hydrogenation step. According to the literature, iron carbides represent the active phase for hydrocarbon formation and are claimed to emerge in the presence of CO. We propose nanostructured FeOx films as model systems to assess information about the complex phase transformations during CO2-FTS. Mesoporous hematite, ferrihydrite, maghemite, maghemite/magnetite films were exposed to CO2-FTS atmospheres at 20 bar and 300°C. Up to three distinct phases were observed depending on the timeon-stream (TOS): a sintered maghemite/magnetite phase, a carbidic core-shell structure, and a low-crystalline, needle-type oxide phase. Our findings indicate that the formation of an intermediary maghemite/magnetite phase, predominant after short TOS (30 h), precedes the evolution of the carbide phase. Yet, even after prolonged TOS (185 h), no full conversion into a bulk carbide is observed. KW - Nanostructured FeOx films KW - CO2 KW - Scanning Auger Spectroscopy PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-549709 DO - https://doi.org/10.1002/cctc.202200240 SN - 1867-3880 VL - 14 IS - 14 SP - 1 EP - 11 PB - Wiley-VCH AN - OPUS4-54970 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Geburtig, Anja A1 - Wachtendorf, Volker A1 - Falkenhagen, Jana T1 - Combined impact of UV radiation and nitric acid on high‐density polyethylene containers as a laboratory test N2 - In a laboratory test, transparent high‐density polyethylene (HDPE) jerrycans have been exposed to both UV radiation and 55 wt‐% nitric acid solution at (41 ± 2)°C, for up to 20 days. For comparison, UV radiant exposure (21 days) and nitric acid exposure (up to 6 weeks) were performed separately, at nearly equal temperatures. The damages are compared with FTIR spectroscopy in ATR and HT‐gel permeation chromatography(GPC) on a molecular level and with hydraulic internal pressure testing as a component test. For the used jerrycans, relevant oxidation can only be found after the combined exposure. This is caused by the decomposition of nitric acid into nitrous gases by UV radiation, which is also observed at lower concentrations (28 wt‐%). After 6 days of laboratory exposure, this is rated as critical, which corresponds to about 1/10 year in Central Europe, according to the UV radiant exposure. The gradual increase in oxidative damage shows the reproducibility of the test. KW - Molecular mass distribution KW - High-density polyethylene KW - Nitric acid KW - UV radiation PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-550141 DO - https://doi.org/10.1002/pts.2673 SN - 0894-3214 SP - 1 EP - 7 PB - John Wiley & Sons Ltd AN - OPUS4-55014 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Chinnasamy, R. A1 - Ravi, J. A1 - Pradeep, V.V. A1 - Manoharan, D. A1 - Emmerling, Franziska A1 - Bhattacharya, Biswajit A1 - Ghosh, S. T1 - Adaptable Optical Microwaveguides From Mechanically Flexible Crystalline Materials N2 - Flexible organic crystals (elastic and plastic) are important materials for optical waveguides, tunable optoelectronic devices, and photonic integrated circuits. Here, we present highly elastic organic crystals of a Schiff base, 1-((E)-(2,5-dichlorophenylimino)methyl)naphthalen-2-ol (1), and an azine molecule, 2,4-dibromo-6-((E)-((E)-(2,6-dichlorobenzylidene)hydrazono)methyl)phenol (2). These microcrystals are highly flexible under external mechanical force, both in the macroscopic and the microscopic regimes. The mechanical flexibility of these crystals arises as a result of weak and dispersive C−H⋅⋅⋅Cl, Cl⋅⋅⋅Cl, Br⋅⋅⋅Br, and π⋅⋅⋅π stacking interactions. Singly and doubly-bent geometries were achieved from their straight shape by a micromechanical approach using the AFM cantilever tip. Crystals of molecules 1 and 2 display a bright-green and red fluorescence (FL), respectively, and selective reabsorption of a part of their FL band. Crystals 1 and 2 exhibit optical-path-dependent low loss emissions at the termini of crystal in their straight and even in extremely bent geometries. Interestingly, the excitation position-dependent optical modes appear in both linear and bent waveguides of crystals 1 and 2, confirming their light-trapping ability. KW - Crystal growth KW - Fluorescence KW - Mechanophotonics KW - Micromanipulation KW - Optical waveguides PY - 2022 DO - https://doi.org/10.1002/chem.202200905 SN - 0947-6539 SP - 1 EP - 8 PB - Wiley VHC-Verlag AN - OPUS4-55018 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Müller, Anja T1 - Determination of the actual morphology of core-shell nanoparticles by advanced X-ray analytical techniques: A necessity for targeted and safe nanotechnology N2 - Even though we often do not knowingly recognize them, nanoparticles are present these days in most areas of our daily life, including food and its packaging, medicine, pharmaceuticals, cosmetics, pigments as well as electronic products, such as computer screens. The majority of these particles exhibits a core-shell morphology either intendedly or unintendedly. For the purpose of practicability, this core-shell nanoparticle (CSNP) morphology is often assumed to be ideal, namely a spherical core fully encapsulated by a shell of homogeneous thickness with a sharp interface between core and shell material. It is furthermore widely presumed that all nanoparticles in the sample possess the same shell thickness. As a matter of fact, most real CSNPs deviate in several ways from this ideal model with quite often severe impact on how efficiently they perform in a specific application. The topic of this cumulative PhD thesis is the accurate characterization of the actual morphology of CSNPs by advanced X-ray analytical techniques, namely X-ray photoelectron spectroscopy (XPS) and scanning transmission X-ray microscopy (STXM). A special focus is on CSNPs which deviate from an ideal core-shell morphology. In the paper from 2019 nanoparticle shell thicknesses are extracted from the elastic-peak intensities in an XPS spectrum based on an ideal particle morphology. This happens for a series of CSNP samples comprising a poly(tetrafluoroethylene) (PTFE) core and either a poly(methyl methacrylate) (PMMA) or polystyrene (PS) shell. The same paper as well as the paper from 2020 demonstrate for the first time, that the analysis of the inelastic background in an XPS spectrum of CSNPs can identify and quantify the heterogeneity of the shell and the incomplete encapsulation of the core. The result from an XPS experiment is always an average across a large nanoparticle ensemble. Deviations from an ideal morphology within a single particle of the sample cannot be assessed separately. As opposed to that, a spatial resolution of 35 nm enables STXM to visualize the interior of single CSNPs which exhibit a sufficient X-ray absorption contrast between core and shell material. In the paper from 2018 a STXM analysis is demonstrated based on the example of the PTFE-PS CSNP samples already mentioned in the previous paragraph. In the publication from 2021 (Ca/Sr)F₂ core-shell like nanoparticle ensembles for the practical use in, among others, antireflective coatings are investigated. These nanoparticles do not possess a sharp interface between core and shell material, which is why a shell thickness determination as described in the second paragraph is inappropriate. Instead, in-depth profiles of the chemical composition are obtained by XPS experiments based on synchrotron radiation with variable X-ray photon energy to elucidate the internal morphology of the particles. Additionally, theoretical in-depth profiles of Ca and Sr XPS peak intensities are simulated, in order to facilitate the interpretation of the experiments. Thus, an enrichment of CaF₂ at the particle surface was determined, which could hardly have been assessed by any other analytical technique. Because this kind of non-destructive depth profiling by XPS is very demanding, more than usual effort is spent on gapless documentation of the experiments to ensure full reproducibility. Due to the vast diversity of nanoparticles differing in material, composition and shape, a measurement procedure cannot unalteredly be transferred from one sample to another. Nevertheless, because the papers in this thesis present a greater depth of reporting on the experiments than comparable publications, they constitute an important guidance for other scientists on how to obtain meaningful information about CSNPs from surface analysis. N2 - Obwohl wir sie oft nicht bewusst wahrnehmen, sind Nanopartikel heutzutage in den meisten Bereichen unseres Alltags präsent, unter anderem in Lebensmitteln und ihren Verpackungen, Medizin, Medikamenten, Kosmetik, Pigmenten und in elektronischen Geräten wie Computermonitoren. Ein Großteil dieser Partikel weist, beabsichtigt oder unbeabsichtigt, eine Kern-Schale Morphologie auf. Einfachheitshalber wird diese Morphologie eines Kern-Schale-Nanopartikels (CSNP) oft als ideal angenommen, d.h. als ein sphärischer Kern, der komplett von einer Schale homogener Dicke bedeckt ist, mit einer scharfen Grenzfläche zwischen Kern- und Schalenmaterial. Außerdem wird vielfach auch davon ausgegangen, alle Partikel der Probe hätten gleiche Schalendicken. Tatsächlich weichen die meisten realen CSNPs in verschiedenster Weise von diesem Idealmodell ab, mit oft drastischen Auswirkungen darauf, wie gut sie ihre Aufgabe in einer bestimmten Anwendung erfüllen. Das Thema dieser kumulativen Doktorarbeit ist die exakte Charakterisierung der wirklichen Morphologie von CSNPs mit modernen Röntgen-basierten Methoden, konkret Röntgen-Photoelektronen-Spektroskopie (XPS) und Raster-Transmissions-Röntgen-Mikroskopie (STXM). Der Fokus liegt insbesondere auf CSNPs, die von einer idealen Kern-Schale-Morphologie abweichen. Im Artikel von 2019 werden Schalendicken von Nanopartikeln aus den elastischen Peakintensitäten im XPS-Spektrum unter Annahme einer idealen Partikelmorphologie abgeleitet. Dies geschieht für eine Reihe von CSNP-Proben, welche aus einem Polytetrafluoroethylen- (PTFE) Kern und entweder einer Polymethylmethacrylat- (PMMA) oder Polystyrol- (PS) Schale bestehen. Sowohl dieser Artikel als auch der von 2020 zeigen erstmals, dass die Auswertung des inelastischen Untergrunds eines CSNP-XPS-Spektrums in der Lage ist, die Heterogenität der Schale und die unvollständige Ummantelung des Kerns zu identifizieren und zu quantifizieren. Das Ergebnis eines XPS-Experiments ist immer ein Mittelwert über ein großes Nanopartikelensemble. Inwiefern ein einzelner Partikel innerhalb der Probe von einer idealen Morphologie abweicht, kann nicht gesondert erfasst werden. Im Gegensatz dazu kann STXM mit einer räumlichen Auflösung von 35 nm das Innere einzelner CSNPs visualisieren, sofern sie genügend Röntgenabsorptionskontrast zwischen Kern- und Schalenmaterial aufweisen. Im Artikel von 2018 wird am Beispiel der bereits im vorherigen Abschnitt genannt PTFE-PS-CSNPProben eine solche STXM-Untersuchung demonstriert. In der Veröffentlichung von 2021 werden Kern-Schale-artige (Ca/Sr)F₂-Nanopartikel für den praktischen Einsatz in unter anderem entspiegelnden Beschichtungen untersucht. Da hier keine scharfe Grenzfläche zwischen Kern- und Schalenmaterial vorliegt, ist eine Schalendickenbestimmung, wie sie im zweiten Abschnitt diskutiert wird, nicht sinnvoll. Stattdessen werden mit Hilfe von XPS, angeregt mit Synchrotronstrahlung bei variabler Röntgenphotonenenergie, Tiefenprofile der chemischen Zusammensetzung generiert, um die innere Morphologie der Partikel aufzuklären. Zusätzlich werden theoretische Tiefenprofile der Ca- und Sr-XPS-Peakintensitäten simuliert, um die Interpretation der Experimente zu erleichtern. So wurde eine CaF₂-Anreicherung an der Oberfläche der Partikel festgestellt, die kaum mit einer anderen analytischen Methode hätte entdeckt werden können. Da diese zerstörungsfreie Bestimmung von XPS-Tiefenprofilen sehr anspruchsvoll ist, wird noch mehr als üblich auf die lückenlose Dokumentation des Experiments geachtet, um vollständige Reproduzierbarkeit zu gewährleisten. Aufgrund der enormen Vielfalt an CSNPs, die sich in Material, Zusammensetzung und Form unterscheiden, kann eine Messmethode nicht völlig unverändert von einer Probe auf eine andere übertragen werden. Nichtsdestotrotz, da die als Teil dieser Doktorarbeit präsentierten Artikel eine deutlich ausführlichere Beschreibung der Experimente enthalten als vergleichbare Publikationen, stellen sie eine wichtige Anleitung für andere Wissenschaftler dafür dar, wie aussagekräftige Informationen über CSNPs durch Oberflächenanalytik erhalten werden können. KW - Core-shell nanoparticle (CSNP) KW - X-ray photoelectron spectroscopy (XPS) KW - Scanning transmission X-ray microscopy (STXM) PY - 2022 DO - https://doi.org/10.18452/24312 SP - i EP - 243 PB - Humboldt-Universität CY - Berlin AN - OPUS4-54991 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Kai A1 - Mirabella, Francesca A1 - Mezra, Marek A1 - Weise, Matthias A1 - Wasmuth, Karsten A1 - Hertwig, Andreas A1 - Krüger, Jörg A1 - Bonse, Jörn A1 - Hodoroaba, Vasile-Dan T1 - ToF-SIMS as a new tool for nano-scale investigation of ps-laser generated surface structures on Titanium substrates N2 - The fabrication of laser-generated surface structures on titanium and titanium alloys has recently gained remarkable interests, being technologically relevant for applications in optics, medicine, fluid transport, tribology, and wetting of surfaces. The morphology of these structures, and so their chemistry, is influenced by the different laser processing parameters such as the laser fluence, wavelength, pulse repetition rate, the effective number of laser pulses per beam spot area, etc. A simple way to characterize laser-generated surface structures is by means of optical microscopy (OM) or white light interference microscopy (WLIM). The latter can address the surface topography, while having a lateral resolution limit of ~(lambda)/2 (lambda = illumination wavelength). To resolve morphologies with spatial periods significantly smaller than (lambda)/2, scanning electron microscopy (SEM) is often used, taking benefit of the reduced de Broglie wavelength associated to the electrons of several keV energy. However, all the above-mentioned techniques lack the necessary depth-resolution to reveal and quantify sub-surface material modifications of these laser-generated structures. Time-of-Flight secondary ion mass spectrometry (ToF-SIMS) represents a promising surface analytical technique for studying laser-induced chemical surface alterations since the method combines a high surface sensitivity with the capability to perform a depth-profiling of the laser-affected surface zone. In this study we combine WLIM and high-resolution SEM with ToF-SIMS to fully characterize the evolution of various types of laser-generated micro- and nanostructures formed on Ti-6Al-4V alloys upon irradiation by near infrared ultrashort laser pulses (1030 nm, 925 fs) at different laser fluence levels, effective number of pulses, and at different pulse repetition rates (1 – 400 kHz). We show how this combined surface analytical approach allows to evaluate alterations in the surface chemistry and topography of the laser-generated surface structures depending on the laser processing parameters T2 - ECASIA 2022 CY - Limerick, Ireland DA - 29.05.2022 KW - Laser-induced periodic surface structures KW - Time of Flight - Secondary ion mass spectrometry KW - White light interferometric microscopy KW - Titanium alloy PY - 2022 AN - OPUS4-54992 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Belenguer, A. A1 - Lampronti, G. A1 - Michalchuk, Adam A1 - Emmerling, Franziska A1 - Sanders, J. T1 - Quantitative reversible one pot interconversion of three crystalline polymorphs by ball mill grinding N2 - We demonstrate here using a disulfide system the first example of reversible, selective, and quantitative transformation between three crystalline polymorphs by ball mill grinding. This includes the discovery of a previously unknown polymorph. Each polymorph is reproducibly obtained under well-defined neat or liquid-assisted grinding conditions, revealing subtle control over the apparent thermodynamic stability. We discovered that the presence of a contaminant as low as 1.5% mol mol−1 acting as a template is required to enable all these three polymorph transformations. The relative stabilities of the polymorphs are determined by the sizes of the nanocrystals produced under different conditions and by surface interactions with small amounts of added solvent. For the first time, we show evidence that each of the three polymorphs is obtained with a unique and reproducible crystalline size. This mechanochemical approach gives access to bulk quantities of metastable polymorphs that are inaccessible through recrystallisation. KW - Mechanochemistry KW - Polymorph KW - XRD PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-549934 DO - https://doi.org/10.1039/D2CE00393G SP - 1 EP - 7 PB - Royal Society of Chemistry AN - OPUS4-54993 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Weidner, Steffen A1 - Meyer, A. A1 - Kricheldorf, H. R. T1 - Sn(II)2-ethylhexanoate-catalyzed polymerizations of L-lactide in solution – Solution grown crystals of cyclic Poly(L-Lactide)s N2 - L-lactide (LA) was polymerized in toluene by means of neat tin(II) 2-ethylhexanoate (SnOct2). Concentration, time and temperature were varied. The isothermally crystallized polyLAs (PLA) were characterized in the virgin state with regard to topology, molar mass, melting temperature (Tm), crystal modification, high or low Tm morphology, crystallinity and crystal thickness. Even a small amount of solvent favored cyclization relative to polymerization in bulk, so that cyclic polylactides were obtained at 115 ◦C and even at 95 ◦C. At all temperatures the α-modification of PLA was obtained along with crystallinities up to 90%. With 6 M solution the high Tm morphology with Tm’s > 190 ◦C was obtained at 115 ◦C. The crystal thickness of crystallites grown from solution at 115 ◦C was on the average 10–20% higher than that of PLA polymerized in bulk. At a polymerization temperature of 75 ◦C cyclization was incomplete and fewer perfect crystallites were formed. A new hypothesis for the crystal growth of cyclic polyLAs is proposed. KW - Polylactide KW - MALDI-TOF MS KW - Crystalinity KW - Polymerization PY - 2022 DO - https://doi.org/10.1016/j.polymer.2022.125142 SN - 0032-3861 VL - 255 SP - 1 EP - 9 PB - Elsevier CY - Oxford AN - OPUS4-55283 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Karafiludis, Stephanos A1 - Stawski, Tomasz T1 - Trash to treasure: recovery of transition metal phosphates for (electro-)catalytical applications N2 - Wastewaters containing high concentrations of NH4+, PO43- and transition metals are environmentally harmful and toxic pollutants. At the same time phosphorous and transition metals constitute valuable resources. Here, we report the synthesis routes for Co- and Ni-struvites (NH4MPO4∙6H2O, M = Ni2+, Co2+) out of aqueous solutions resembling synthetic/industrial waste water compositions, and allowing for P, ammonia and metal co-precipitation. Furthermore, the as-obtained struvites were further up-cycled. When heated, these transition metal phosphates (TMPs) demonstrate significant changes in the degree of crystallinity/coordination environment involving a high amount of amorphous phases and importantly develop mesoporosity (Figure 1). In this regard, amorphous and mesoporous TMPs are known to be highly promising (electro-)catalysts. Amorphous phases do not represent a simple “disordered” crystal but more a complex system with a broad range of compositions and physicochemical properties, which remain mostly unknown. Consequently, we investigated the recrystallization and amorphization process during thermal treatment and a resolved the complex amorphous/crystalline structures (Figure 2). As a proof-of-principle for their applicational use, the as-obtained TMPs demonstrate significant proton conductivity properties similar to apatite-like structures from room to high temperatures (>800°C). Hence, we have developed a promising recycling route in which environmental harmful contaminants like PO43-, NH4+ and 3d metals would be extracted out of waste waters in the form of precursor raw materials. These raw materials can be then further up-cycled through a simple thermal treatment for their specific application in electrocatalysis. T2 - Goldschmidt Conference 2022 CY - Hawai'i, USA DA - 10.07.2022 KW - Mesoporosity KW - Amorphous phases KW - Transition metals KW - Struvite KW - Phosphates PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-552852 UR - https://conf.goldschmidt.info/goldschmidt/2022/meetingapp.cgi/Paper/9501 AN - OPUS4-55285 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Karafiludis, Stephanos A1 - de Oliveira Guilherme Buzanich, Ana A1 - Kochovski, Z. A1 - Feldmann, Ines A1 - Emmerling, Franziska A1 - Stawski, Tomasz T1 - Ni- and Co-Struvites: Revealing Crystallization Mechanisms and Crystal Engineering toward Applicational Use of Transition Metal Phosphates N2 - Industrial and agricultural waste streams (waste water, sludges, tailings, etc.) which contain high concentrations of NH4+, PO43–, and transition metals are environmentally harmful and toxic pollutants. At the same time, phosphorous and transition metals constitute highly valuable resources. Typically, separate pathways have been considered to extract hazardous transition metals or phosphate independently from each other. Investigations on the simultaneous removal of multiple components have been carried out only to a limited extent. Here, we report the synthesis routes for Ni- and Co-struvites (NH4MPO4·6H2O, M = Ni2+ and Co2+), which allow for P, ammonia, and metal co-precipitation. By evaluating different reaction parameters, the phase and stability of transition metal struvites as well as their crystal morphologies and sizes could be optimized. Ni-struvite is stable in a wide reactant concentration range and at different metal/phosphorus (M/P) ratios, whereas Co-struvite only forms at low M/P ratios. Detailed investigations of the precipitation process using ex situ and in situ techniques provided insights into the crystallization mechanisms/crystal engineering of these materials. M-struvites crystallize via intermediate colloidal amorphous nanophases, which subsequently aggregate and condense to final crystals after extended reaction times. However, the exact reaction kinetics of the formation of a final crystalline product varies significantly depending on the involved metal cation in the precipitation process: several seconds (Mg) to minutes (Ni) to hours (Co). The achieved level of control over the morphology and size makes precipitation of transition metal struvites a promising method for direct metal recovery and binding them in the form of valuable phosphate raw materials. Under this paradigm, the crystals can be potentially up-cycled as precursor powders for electrochemical or (electro)catalytic applications, which require transition metal phosphates. KW - Crystallization KW - Struvite KW - Nickel KW - Cobalt KW - Phosphorous recovery KW - Up-cycling KW - Aqueous synthesis PY - 2022 DO - https://doi.org/10.1021/acs.cgd.2c00284 VL - 22 IS - 7 SP - 4305 EP - 4315 PB - ACS Publications CY - Washington D.C. AN - OPUS4-55286 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lilensten, L. A1 - Provost, K. A1 - Perrière, L. A1 - Fonda, E. A1 - Couzinié, J. A1 - Amman, F. A1 - Radtke, Martin A1 - Dirras, G. A1 - Guillot, I. T1 - Experimental investigation of the local environment and lattice distortion in refractory medium entropy alloys N2 - EXAFS analysis of pure elements, binary and ternary equiatomic refractory alloys within the Nb-Zr-Ti-Hf- Ta system is performed at the Nb and Zr K-edges to analyze the evolution of the chemical local environ- ment and the lattice distortion. A good mixing of the elements is found at the atomic scale. For some compounds, a distribution of distances between the central atom and its neighbors suggests a distortion of the structure. Finally, analysis of the Debye-Waller parameters shows some correlation with the lat- tice distortion parameter δ², and allows to quantify experimentally the static disorder in medium entropy alloys. KW - BAMline KW - Refractory alloys KW - EXAFS KW - Debye-Waller parameter PY - 2022 DO - https://doi.org/10.1016/j.scriptamat.2022.114532 SN - 1359-6462 VL - 211 SP - 1 EP - 6 PB - Elsevier Ltd. AN - OPUS4-55287 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Margreiter, R. A1 - Baumann, J. A1 - Mantouvalou, I. A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Strub, E. T1 - Investigations on fire-gilding N2 - Fire-gilding is a historic technique for the application of golden layers on a number of different base materials utilizing a gold amalgam. This technique leaves a significant amount of Hg in the golden layer, giving archeometrists a reliable indicator to identify firegildings. Recent findings on presumably fire-gilded objects have shown in several cases significantly lower Hg content than previously studied objects. This prompted a synchrotron-based X-ray fluorescence investigation into the Hg distribution along the material–gilding interface, as well as a series of measurements regarding the Hg content development in fire-gilded samples during artificial aging. This work presents findings on laboratory-prepared fire-gildings, indicating an Hg enrichment at the interface of firegilded silver samples. Notably, such an enrichment is missing in fire-gilded copper samples. Further, it is confirmed that fire-gilded layers typically do not undercut an Hg bulk content of 5%. In this light, it seems improbable that ancient samples that contain <5% Hg are fire-gilded. The results presented in this study might lead to a non-destructive method to identify the Hg enrichment at the interface. This might be obtained by a combination of different non-destructive measurements and might also work unambiguously in samples in which the gold top layer is altered. KW - BAMline KW - X-Ray Fluorescence KW - Gilding KW - Depth profile KW - Archaeometry PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-552885 DO - https://doi.org/10.1111/arcm.12797 SN - 0003-813X SP - 1 EP - 14 PB - Wiley online library AN - OPUS4-55288 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dietrich, P. M. A1 - Kjærvik, Marit A1 - Willneff, E. A. A1 - Unger, Wolfgang T1 - In-depth analysis of iodine in artificial biofilm model layers by variable excitation energy XPS and argon gas cluster ion sputtering XPS N2 - Here, we present a study on agarose thin-film samples that represent a model system for the exopolysaccharide matrix of biofilms. Povidone-iodide (PVP-I) was selected as an antibacterial agent to evaluate our x-ray photoelectron spectroscopy (XPS)-based methodology to trace specific marker elements, here iodine, commonly found in organic matrices of antibiotics. The in-depth distribution of iodine was determined by XPS analyses with variable excitation energies and in combination with argon gas cluster ion beam sputter cycles. On mixed agarose/PVP-I nanometer-thin films, both methods were found to solve the analytical task and deliver independently comparable results. In the mixed agarose/PVP-I thin film, we found the outermost surface layer depleted in iodine, whereas the iodine is homogeneously distributed in the depth region between this outermost surface layer and the interface between the thin film and the substrate. Depletion of iodine from the uppermost surface in the thin-film samples is assumed to be caused by ultrahigh vacuum exposure resulting in a loss of molecular iodine (I2) as reported earlier for other iodine-doped polymers. KW - Biofilm KW - XPS KW - Argon gas cluster ion sputtering KW - Variable excitation KW - Iodine PY - 2022 DO - https://doi.org/10.1116/6.0001812 SN - 1934-8630 VL - 17 IS - 3 SP - 1 EP - 8 PB - AVS AN - OPUS4-54973 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Chabbah, T. A1 - Chatti, S. A1 - Zouaoui, F. A1 - Jlalia, A. A1 - Gaiji, H. A1 - Abderrazak, H. A1 - Casablanca, H. A1 - Mercier, R. A1 - Weidner, Steffen A1 - Errachid, A. A1 - Marestin, C. A1 - Jaffrezic-Renault, N. T1 - New poly(ether-phosphoramide)s sulfides based on green resources as sensitive films for the specific impedimetric detection of nickel ions N2 - For the development of selective and sensitive chemical sensors, we have developed a new family of poly(etherphosphoramide) polymers. These polymers were obtained with satisfactory yields by nucleophilic aromatic polycondensation using isosorbide as green resources, and bisphenol A with two novel difluoro phosphinothioic amide monomers. Unprecedented, the thiophosphorylated aminoheterocycles monomers, functionalized with two heterocyclic amine, N-methylpiperazine and morpholine were successfully obtained by nucleophilic substitution reaction of P(S)–Cl compound. The resulting polymers were characterized by different analytical techniques (NMR, MALDI–ToF MS, GPC, DSC, and ATG). The resulting partially green polymers, having tertiary phosphine sulfide with P–N side chain functionalities along the main chain of polymers are the sensitive film at the surface of a gold electrode for the impedimetric detection of Cd, Ni, Pb and Hg. The bio-based poly(etherphosphoramide) functionalized with N-methylpiperazine modified sensor showed better analytical performance than petrochemical based polymers for the detection of Ni2+. A detection limit of 50 pM was obtained which is very low compared to the previously published electrochemical sensors for nickel detection. KW - Poly(ether-phosphoramide)s sulfides KW - Green chemistry KW - Polymer film KW - MALDI TOF MS PY - 2022 DO - https://doi.org/10.1016/j.talanta.2022.123550 VL - 247 IS - 123550 SP - 1 EP - 9 PB - Elsevier B.V. AN - OPUS4-54980 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - VIDEO A1 - Schwibbert, Karin A1 - Richter, Anja A1 - Bonse, Jörn T1 - BioCombs4Nanofibers: From nanofibers over spiders to bacteria N2 - This 6 minute long MP4-video presents some key results of the European research project "BioCombs4Nanofibers" to the broader public. Inspired by nature, some concepts of certain types of spiders are transferred to technology in order to develop bacteria-repellent surfaces through laser surface nanostructuring. Funding notice: This study was funded by the European Union's research and innovation program under the FET Open grant agreement No. 862016 (BioCombs4Nanofibers, http://biocombs4nanofibers.eu). KW - Antiadhesive surfaces KW - Laser-induced periodic surface structures (LIPSS) KW - Cribellate spiders KW - Bacterial adhesion tests KW - Bacteria-repellent surfaces PY - 2022 UR - https://download.jku.at/org/7kM/xyU/BioCombs4Nanofibers/D5.6_video%20for%20the%20broader%20public_23.03.2022.mp4 UR - https://www.jku.at/en/biocombs4nanofibers/dissemination/ DO - https://doi.org/10.26272/opus4-54939 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-54939 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bresch, Harald A1 - Hodoroaba, Vasile-Dan A1 - Schmidt, Alexandra A1 - Rasmussen, K. A1 - Rauscher, H. T1 - Counting Small Particles in Electron Microscopy Images — Proposal for Rules and Their Application in Practice N2 - Electron microscopy (EM) is the gold standard for the characterisation of the morphology (size and shape) of nanoparticles. Visual observation of objects under examination is always a necessary first step in the characterisation process. Several questions arise when undertaking to identify and count particles to measure their size and shape distribution. In addition to challenges with the dispersion and identification of the particles, more than one protocol for counting particles is in use. This paper focuses on precise rules for the counting of particles in EM micrographs, as this influences the measurement accuracy of the number of particles, thus implicitly affecting the size values of the counted particles. We review and compare four different, commonly used methods for counting, which we then apply in case studies. The impact of the selected counting rule on the obtained final particle size distribution is highlighted. One main aim of this analysis is to support the application of a specific, well-defined counting approach in accordance with regulatory requirements to contribute to achieving more reliable and reproducible results. It is also useful for the new harmonised measurement procedures for determining the particle size and particle size distribution of nanomaterials. KW - Nano KW - Particle size distribution KW - Nanoparticle KW - Nanomaterial KW - OECD PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-551891 DO - https://doi.org/10.3390/nano12132238 SN - 2079-4991 VL - 12 IS - 13 SP - 2238 PB - MDPI CY - Basel AN - OPUS4-55189 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kolmangadi, Mohamed Aejaz A1 - Smales, Glen Jacob A1 - ZhuoQing, Li A1 - Yildirim, Arda A1 - Wuckert, E. A1 - Eutionnat, S. A1 - Demel, F. A1 - Huber, P A1 - Lasachat, S. A1 - Schönhals, Andreas T1 - Side Chain Length-Dependent Dynamics and Conductivity in Self-Assembled Ion N2 - We study the molecular mobility and electrical conductivity of a homologous series of linear shaped columnar ionic liquid crystals ILCn, (n = 8, 10, 12, 14, 16) using broadband dielectric spectroscopy (BDS), specific heat spectroscopy (SHS), and X-ray scattering. We aim to understand how the alkyl chain length influences the dynamics and electric conductivity in this system. Two dielectrically active relaxation modes are observed, the γ and the αcore process, that correspond to the localized fluctuations of the alkyl chains and cooperative motions of the aromatic core in the columns, respectively. Both the γ relaxation and the αcore process slow down with increasing alkyl chain length. SHS reveals one relaxation process, the αalkyl process that has a similar temperature dependence as that of the αcore process for ILC12, 14, and 16 but shifts to higher temperature for ILC8 and 10. For ILC12, 14, and 16, the absolute values of DC conductivity increase by 4 orders of magnitude at the transition from the plastic crystalline to hexagonal columnar phase. For ILC8 and 10, the DC conductivity behavior is similar to ionic liquids, where the conductivity is coupled with structural relaxation. Small-angle X-ray investigations reveal that both the intercolumnar distance and the disorder coherence length increase with alkyl chain length; conversely, the DC conductivity decreases monotonically. KW - Ionic Liquid Crystals PY - 2022 DO - https://doi.org/10.1021/acs.jpcc.2c03023 SN - 1932-7447 VL - 126 IS - 27 SP - 10995 EP - 11006 PB - ACS AN - OPUS4-55194 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stawski, Tomasz A1 - Wolf, Jakob A1 - Emmerling, Franziska T1 - Smart Machines, New Materials, Automated Future N2 - In pursuing the automated synthesis of metal nanoparticles (NPs), the capabilities of the “Chemputer” are deployed, for the first time, into the field of inorganic chemistry. Metal NPs have a substantial impact across different fields of science, such as photochemistry, energy conversion, and medicine. Among the commonly used nanoparticles, silver NPs are of special interest due to their antibacterial properties and applications in sensing and catalysis. However, many of the methods used to synthesize Ag NPs often do not result in well-defined products, the main obstacles being high polydispersity or a lack of particle size tunability. The Chemputer is a modular, automated platform developed by the Cronin group for execution of multi-step, solution based organic synthesis. The machine has been further implemented at BAM, where we used this setup to perform automated organic syntheses, autonomously controlled by feedback derived from online NMR. In the Chemputer liquids can be transferred across a backbone, constructed from HPLC selection valves and syringe pumps. The Chemputer operates in a batch mode, common laboratory devices, such as heaters and glassware like round bottom flasks, are connected to the backbone, forming reaction modules. Solutions can be manipulated in these modules, and as all operations are controlled through a software script, reproducibility among individual syntheses is high. Likewise, any adjustments of the synthesis conditions, if required, are straightforward to implement and are documented in the reaction log file and a code versioning system. We characterised Chemputer-synthesized nanoparticles using small-angle X-ray scattering, dynamic light scattering and further methods, showing that automated synthesis can yield colloids with reproducible and tuneable properties. The approach is an important first step towards the automation of nanoparticle syntheses in a modular, multipurpose platform. The modularity of the Chemputer opens many possibilities for the synthesis of a variety of different NP morphologies and sizes and potentially more complex structures. These advances and further work can help in the general investigations of silver nanoparticles by supplying a reliable and reproducible method of their synthesis and removing tacit knowledge by significantly reducing the experimental bias. T2 - Analytica 2022 CY - Munich, Germany DA - 21.06.2022 KW - Automated synthesis KW - Nanoparticles PY - 2022 AN - OPUS4-55198 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kittner, Maria A1 - Kerndorff, A. A1 - Ricking, M. A1 - Bednarz, M. A1 - Obermaier, N. A1 - Lukas, M. A1 - Asenova, M. A1 - Bordós, G. A1 - Eisentraut, Paul A1 - Hohenblum, P. A1 - Hudcova, H. A1 - Humer, F. A1 - István, T. G. A1 - Kirchner, M. A1 - Marushevska, O. A1 - Nemejcová, D. A1 - Oswald, P. A1 - Paunovic, M. A1 - Sengl, M. A1 - Slobodnik, J. A1 - Spanowsky, K. A1 - Tudorache, M. A1 - Wagensonner, H. A1 - Liska, I. A1 - Braun, U. A1 - Bannick, C. G. T1 - Microplastics in the Danube River Basin: A First Comprehensive Screening with a Harmonized Analytical Approach N2 - In this study, carried out within the Joint Danube Survey 4, a comprehensive microplastic screening in the water column within a large European river basin from its source to estuary, including major tributaries, was realized. The objective was to develop principles of a systematic and practicable microplastic monitoring strategy using sedimentation boxes for collection of suspended particulate matter followed by its subsequent analysis using thermal extraction desorption-gas chromatography/mass spectrometry. In total, 18 sampling sites in the Danube River Basin were investigated. The obtained suspended particulate matter samples were subdivided into the fractions of >100 μm and <100 μm and subsequently analyzed for microplastic mass contents. The results showed that microplastics were detected in all samples, with polyethylene being the predominant polymer with maximum contents of 22.24 μg/mg, 3.23 μg/mg for polystyrene, 1.03 μg/mg for styrene-butadiene-rubber, and 0.45 μg/mg for polypropylene. Further, polymers such as different sorts of polyester, polyacrylates, polylactide, and natural rubber were not detected or below the detection limit. Additional investigations on possible interference of polyethylene signals by algae-derived fatty acids were assessed. In the context of targeted monitoring, repeated measurements provide more certainty in the interpretation of the results for the individual sites. Nevertheless, it can be stated that the chosen approach using an integrative sampling and determination of total plastic content proved to be successful. KW - Thermal extraction desorption-gas chromatography/mass spectrometry (TED-GC/MS), monitoring KW - Microplastics KW - River KW - Suspended particulate matter (SPM) KW - Sedimentation box (SB) PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-551444 DO - https://doi.org/10.1021/acsestwater.1c00439 VL - 2 IS - 7 SP - 1174 EP - 1181 PB - ACS Publications AN - OPUS4-55144 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - George, Janine A1 - Petretto, G. A1 - Naik, Aakash Ashok A1 - Esters, M. A1 - Jackson, A. J. A1 - Nelson, R. A1 - Dronskowski, R. A1 - Rignanese, G.-M. A1 - Hautier, G. T1 - Automated bonding analysis with crystal orbital Hamilton populuations N2 - Automated bonding analysis software has been developed based on Crystal Orbital Hamilton Populations to facilitate high-throughput bonding analysis and machine-learning of bonding features. This work presents the software and discusses its applications to simple and complex materials such as GaN, NaCl, the oxynitrides XTaO2N (X=Ca, Ba, Sr) and Yb14Mn1Sb11. KW - Chemical bonds KW - Automation KW - High-throughput PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-551641 DO - https://doi.org/10.1002/cplu.202200123 SN - 2192-6506 SP - 1 EP - 11 PB - Wiley-VCH CY - Weinheim AN - OPUS4-55164 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - George, Janine T1 - DFT-based Phonon-computations for "Considering the Role of Ion Transport in Diffuson-Dominated Thermal Conductivity" N2 - These are the harmonic phonon and Grüneisen parameter computations for the publication "Considering the Role of Ion Transport in Diffuson-Dominated Thermal Conductivity" (https://doi.org/10.1002/aenm.202200717). VASP and Phonopy outputs are included in this data set. KW - Thermal conductivity KW - Phonons PY - 2021 DO - https://doi.org/10.5281/zenodo.5116360 PB - Zenodo CY - Geneva AN - OPUS4-55168 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - George, Janine A1 - Petretto, G. A1 - Naik, Aakash Ashok A1 - Esters, M. A1 - Jackson, A. J. A1 - Nelson, R. A1 - Dronskowski, R. A1 - Rignanese, G.-M. A1 - Hautier, G. T1 - Automated bonding analysis with crystal orbital Hamilton populations (program code LobsterPy) N2 - This is the code for the program LobsterPy that can be used to automatically analyze and plot outputs of the program Lobster. KW - Automation KW - High-throughput computations KW - Bonding analysis PY - 2022 UR - https://doi.org/10.5281/zenodo.6320074 UR - https://doi.org/10.5281/zenodo.6415169 UR - https://doi.org/10.5281/zenodo.6415336 UR - https://doi.org/10.5281/zenodo.6581118 DO - https://doi.org/10.5281/zenodo.6320073 PB - Zenodo CY - Geneva AN - OPUS4-55174 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sachse, René A1 - Hodoroaba, Vasile-Dan A1 - Kraehnert, R. A1 - Hertwig, Andreas T1 - Multilevel effective material approximation for modeling ellipsometric measurements on complex porous thin films N2 - Catalysts are important components in chemical processes because they lower the activation energy and thus determine the rate, efficiency and selectivity of a chemical reaction. This property plays an important role in many of today’s processes, including the electrochemical splitting of water. Due to the continuous development of catalyst materials, they are becoming more complex, which makes a reliable evaluation of physicochemical properties challenging even for modern analytical measurement techniques and industrial manufacturing. We present a fast, vacuum-free and non-destructive analytical approach using multi-sample spectroscopic ellipsometry to determine relevant material parameters such as film thickness, porosity and composition of mesoporous IrOx–TiOy films. Mesoporous IrOx–TiOy films were deposited on Si wafers by sol–gel synthesis, varying the composition of the mixed oxide films between 0 and 100 wt%Ir. The ellipsometric modeling is based on an anisotropic Bruggeman effective medium approximation (a-BEMA) to determine the film thickness and volume fraction of the material and pores. The volume fraction of the material was again modeled using a Bruggeman EMA to determine the chemical composition of the materials. The ellipsometric fitting results were compared with complementary methods, such as scanning electron microscopy (SEM), electron probe microanalysis (EPMA) as well as environmental ellipsometric porosimetry (EEP). KW - Electrochemical catalysts KW - Mixed metal oxide KW - Multi-sample analysis KW - Spectroscopic ellipsometry KW - Thin mesoporous films PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-551026 DO - https://doi.org/10.1515/aot-2022-0007 SN - 2192-8584 SN - 2192-8576 VL - 11 IS - 3-4 (Topical issue: Ellipsometry) SP - 137 EP - 147 PB - De Gruyter CY - Berlin AN - OPUS4-55102 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - George, Janine T1 - Raw data for "Automated bonding analysis with crystal orbital Hamilton populations" N2 - Raw data corresponding to the following paper: 10.1002/cplu.202200123. KW - Automation KW - High-throughput computations KW - Bonding analysis PY - 2022 UR - https://doi.org/10.5281/zenodo.6373369 DO - https://doi.org/10.5281/zenodo.6373368 PB - Zenodo CY - Geneva AN - OPUS4-55175 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - George, Janine A1 - Naik, Aakash Ashok A1 - Jackson, A. J. A1 - Baird, S. T1 - Scripts to reproduce "Automated bonding analysis with crystal orbital Hamilton populations" N2 - This repo allows to recreate our publication: https://doi.org/10.1002/cplu.202200123 In contrast to 0.2.2, we fixed an issue with absolute path. KW - Automation KW - High-throughput computations KW - Bonding analysis PY - 2022 UR - https://github.com/JaGeo/LobsterAutomation UR - https://doi.org/10.5281/zenodo.6421928 UR - https://doi.org/10.5281/zenodo.6595062 UR - https://doi.org/10.5281/zenodo.6599556 UR - https://doi.org/10.5281/zenodo.6674670 UR - https://doi.org/10.5281/zenodo.6704163 DO - https://doi.org/10.5281/zenodo.6421927 PB - Zenodo CY - Geneva AN - OPUS4-55177 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Das, Chayanika A1 - Kastania, Eleni A1 - Witt, Julia A1 - Özcan Sandikcioglu, Özlem T1 - Corrosion protection properties of poly(4-vinyl pyridine) containing multilayer polymeric coatings on magnesium alloy AZ31 N2 - The aim of this study is to develop polymeric thin films for corrosion protection of magnesium alloy AZ31. As polymer matrix, poly(4-vinyl pyridine) (P4VP) is selected due to its semiconducting properties and protonic conductivity. Polyacrylic acid is tested as crosslinking layers to improve interfacial adhesion. The macroscopic corrosion properties of the multilayer coatings are investigated by means of electrochemical methods, such as linear sweep voltammetry and electrochemical impedance spectroscopy (EIS), in corrosive media simulating technical and biomedical applications. It is demonstrated that thin multilayer coatings can suppress the corrosion rates of magnesium alloys. To our best knowledge, this is the first demonstration of the use of P4VP as a conducting polymer film with protonic conductivity for corrosion protection of magnesium alloys. KW - Multilayercoatings KW - AZ31 KW - Corrosion protection KW - Intrinsically conducting polymers KW - Magnesium alloys PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-551799 DO - https://doi.org/10.1002/maco.202112708 SN - 0947-5117 VL - 73 IS - 3 SP - 427 EP - 435 PB - Wiley VHC-Verlag AN - OPUS4-55179 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zvereva, V.V. A1 - Asanov, I.P. A1 - Yusenko, Kirill A1 - Zadesenec, A.V. A1 - Plyusnin, P.E. A1 - Gerasimov, E.Yu. A1 - Maksimovskiy, E.A. A1 - Korenev, S.V. A1 - Asanova, T.I. T1 - Local atomic and electronic structure of Pt‑Os nanoplates and nanofbers derived from the single‑source precursor (NH4)2[Pt0.5Os0.5Cl6] N2 - Abstract Nowadays, Pt-Os binary systems are mainly considered as catalysts and electrocatalysts, but the role of Os in these processes is still poorly understood. The electronic structure of Pt-Os nanosystems remains a few studied as well. Using bimetallic (NH4)2[Pt0.5Os0.5Cl6] as a single-source precursor for preparing Pt-Os nanoalloy through the thermal decomposition in hydrogen and inert atmospheres, the relation of morphology, atomic ordering, and electronic structure of Pt-Os nanoalloy was examined by in situ Quick XAFS, XPS, PXRD, SEM, and HRTEM techniques. Being the only variable parameter, the decomposition atmosphere was found to govern the morphology of the Pt-Os nanoalloy and change the atomic ordering (alloying extent), which involves a change in the electronic structure. In a hydrogen atmosphere, the nanofibers (NFs) (ø ~ 5–6 nm) with the atomic ordering Oscore&Pt-richshell were observed to form; in a nitrogen atmosphere, thin nanoplates (NPLs) (~ 12 nm) with the atomic architecture Os-richcore&Ptrichshell were found out. The depletion in the Os 5d5/2 and Pt 5d5/2,3/2 states was revealed for Pt-Os nanoalloys. This unusual result disagrees with the known d-band theory and indicates that there is a gain of non-d conduction electron counts at one or both sites. Mixed conductivity may exist in such Pt-Os nanoalloy that may be responsible for a manifestation of new physical properties of this binary system . KW - Bimetallic alloy KW - Nanoalloy KW - Synchrotron radiation KW - XAFS KW - Electronic structure KW - Alloy morphology PY - 2021 DO - https://doi.org/10.1007/s11051-021-05378-z SN - 1388-0764 VL - 24 IS - 1 SP - 1 EP - 23 PB - Springer AN - OPUS4-55347 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Accorsi, M. A1 - Tiemann, M. A1 - Wehrhan, L. A1 - Finn, Lauren M. A1 - Cruz, R. A1 - Rautenberg, Max A1 - Emmerling, Franziska A1 - Heberle, J. A1 - Keller, B. G. A1 - Rademann, J. T1 - Pentafluorophosphato-Phenylalanines: Amphiphilic Phosphotyrosine Mimetics Displaying Fluorine-Specific Protein Interactions N2 - Phosphotyrosine residues are essential functional switches in health and disease. Thus, phosphotyrosine biomimetics are crucial for the development of chemical tools and drug molecules. We report here the discovery and investigation of pentafluorophosphato amino acids as novel phosphotyrosine biomimetics. A mild acidic pentafluorination protocol was developed and two PF5-amino acids were prepared and employed in peptide synthesis. Their structures, reactivities, and fluorine-specific interactions were studied by NMR and IR spectroscopy, X-ray diffraction, and in bioactivity assays. The mono-anionic PF5 motif displayed an amphiphilic character binding to hydrophobic surfaces, to water molecules, and to protein-binding sites, exploiting charge and H−F-bonding interactions. The novel motifs bind 25- to 30-fold stronger to the phosphotyrosine binding site of the protein tyrosine phosphatase PTP1B than the best current biomimetics, as rationalized by computational methods, including molecular dynamics simulations. KW - Chemical Biology KW - Drug Development KW - Pentafluorophosphates KW - Phosphotyrosine Biomimetics KW - Protein Tyrosine Phosphatases PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-549984 DO - https://doi.org/10.1002/anie.202203579 SN - 1433-7851 VL - 134 IS - 25 SP - 1 EP - 6 PB - Wiley-VCH GmbH AN - OPUS4-54998 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - George, Janine T1 - Data-driven chemical understanding N2 - Chemical heuristics are essential to understanding molecules and materials in chemistry. The periodic table, atomic radii, and electronegativities are only a few examples. Initially, they have been developed by a combination of physical insight and a limited amount of data. It is now possible to test these heuristics and generate new ones using automation based on Materials Informatic tools like pymatgen and greater amounts of data from databases such as a Materials Project. In this session, I'll speak about heuristics and design rules based on coordination environments and the concept of chemical bonding. For example, we have tested the Pauling rules which describe the stability of materials based on coordination environments and their connections on 5000 oxides from the Materials Project. In addition, we have created automated processes for analyzing the chemical bonding situation in crystalline materials with Lobster (www.cohp.de) in order to discover new heuristics and design rules. T2 - Materials Project Seminar Series CY - Online meeting DA - 18.05.2022 KW - DFT KW - Chemical heuristics KW - Crystal Orbital Hamilton Populations KW - Machine learning KW - Phonons PY - 2022 UR - https://www.youtube.com/watch?v=e7zYrz6fgog UR - https://next-gen.materialsproject.org/community/seminar AN - OPUS4-55008 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Frunza, L. A1 - Zgura, I A1 - Ganea, C. P. A1 - Schönhals, Andreas T1 - Molecular dynamics of alkyl benzoate liquid crystals in the bulk state and in the surface layer of their composites with oxide nanopowders N2 - This paper presents the results concerning monotropic nematic liquid crystals 4-pentylphenyl 40-alkyl benzoate (5PnB) (n = 3 or 5 carbon atoms in the alkyl chain). Their mesophase properties were supported by images of the polarized optical microscopy. Molecular dynamics in the bulk samples or in the composites prepared with aerosil A380 was investigated by broadband dielectric spectroscopy in a large temperature range, appropriately chosen. Thermo gravimetric and infrared investigations were additionally performed. The data were compared with those of structurally related nematics like cyanophenyl pentyl benzoates, which have a cyan group instead of the pentyl chain. The dielectric spectra of the bulk 3P5B and 5P5B demonstrate a dielectric behavior with several relaxation processes as expected for nematic liquid crystals. The temperature dependence of the relaxation rates (and of the dielectric strength) seems to have two distinguished regimes. Thus, in the isotropic state, at higher temperatures the data obey the Vogel–Fulcher–Tammann law, whereas an Arrhenius law is fitted at lower temperature, in a close similarity to the behavior of a constrained dynamic glass transition. Samples with a high density of silica (larger than 7 g aerosil/1 g of 5PnB) were prepared to observe a thin layer adsorbed on the particle surface; it was estimated that almost each guest 5PnB molecule interacts with the aerosil surface. For the composites only one main relaxation process is observed at frequencies much lower than those for the corresponding bulk, which was assigned to the dynamics of the molecules in the surface layer. Infrared spectroscopy shows that these molecules interact with the surface by the ester carbonyl group leading to the monolayer self-assembly at liquid–solid interface. We note once more the importance of the functional unit(s) for the interaction with the hydroxyl groups on the aerosil surface. KW - Liquid crystals PY - 2022 DO - https://doi.org/10.1016/j.molliq.2022.119374 SN - 0167-7322 VL - 359 SP - 1 EP - 11 PB - Elsevier B.V. AN - OPUS4-54867 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bonse, Jörn A1 - Florian, Camilo A1 - Mezera, Marek A1 - Wasmuth, Karsten A1 - Richter, Anja A1 - Schwibbert, Karin A1 - Krüger, Jörg A1 - Müller, F. A. A1 - Gräf, S. T1 - A brief survey on open questions about laser-induced periodic surface structures N2 - The processing of laser-induced periodic surface structures (LIPSS) represents a simple and robust way for the nanostructuring of solids that allows creating a wide range of surface functionalities featuring applications in optics, tribology, medicine, energy technologies, etc. While the currently available laser and scanner technology already allows surface processing rates at the m2/min level, industrial applications of LIPSS are sometimes hampered by the complex interplay between the nanoscale surface topography and the specific surface chemistry. This typically manifests in difficulties to control the processing of LIPSS and in limitations to ensure the long-term stability of the created surface functions. This presentation aims to identify some unsolved scientific problems related to LIPSS, discusses the pending technological limitations, and sketches the current state of theoretical modelling. Hereby, it is intended to stimulate further research and developments in the field of LIPSS for overcoming these limitations and for supporting the transfer of the LIPSS technology into industry. T2 - E-MRS Spring Meeting 2022 CY - Online meeting DA - 30.05.2022 KW - Laser-induced periodic surface structures (LIPSS) KW - Surface functionalization KW - Industrial applications KW - Biofilm growth PY - 2022 AN - OPUS4-54929 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Richter, Anja A1 - Buchberger, G. A1 - Stifter, D. A1 - Duchoslav, J. A1 - Hertwig, Andreas A1 - Bonse, Jörn A1 - Heitz, J. A1 - Schwibbert, Karin T1 - Reducing Escherichia coli adhesion to PET by modulating spatial periods of laser-induced surface nanoripples N2 - Using nanofiber-like cell appendages, secreted proteins and sugars, bacteria can establish initial surface contact followed by irreversible adhesion and the formation of multicellular biofilms. Here, the stabilizing extracellular biofilm matrix together with physiological changes on the single cell level leads to an increased resilience towards harsh environmental conditions, antimicrobials, the host immune response and established cleaning procedures. Persistent microbial adhesion on e.g., medical implants, in water supply networks or food-processing industry is often associated with chronic inflammation, nosocomial and foodborne infections, enhanced biofouling and product contamination. To prevent persistent microbial colonization, antibacterial surface strategies often target the initial steps of biofilm formation and impede adhesion of single cells before a mature biofilm is being formed. While chemical coatings have been widely used, their restricted biocompatibility for eukaryotic cells and attenuated antibacterial-effects due to compound release limit their areas of application and alternative strategies focus on modified surfaces topographies to impede bacterial adhesion. In this work, we used ns-UV laser treatment (wavelength 248 nm and a pulse duration of 20 ns) to generate laser-induced periodic surface structures (LIPSS) with different submicrometric periods ranging from ~210 to ~610 nm on commercial poly(ethylene terephthalate) (PET) foils. Following structurally and chemically analyses, PET samples were subjected to bacterial colonization studies with Escherichia coli TG1, a bacterial test strain with a strong biofilm formation capacity due to the formation of nanofiber-like cell-appendages (pili). Bacterial adhesion tests revealed that E. coli repellence decisively depends on the spatial periods of the LIPSS with the strongest reduction (~91%) in cell adhesion observed for LIPSS periods of 214 nm. Scanning electron microscopy and additional biofilm studies using a pili-deficient E. coli TG1 strain revealed the importance of extracellular appendages in the bacterial repellence observed here, thus, pointing out new antibiotics-free strategies for antibacterial surfaces by impeding nanofiber-mediated bacterial adhesion. T2 - E-MRS Spring Meeting 2022 CY - Online meeting DA - 30.05.2022 KW - Laser-induced periodic surface structures (LIPSS) KW - Bacterial adhesion tests KW - Bacteria repellent surfaces KW - Polymer foils KW - E. coli PY - 2022 AN - OPUS4-54930 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bonse, Jörn A1 - Mirabella, Francesca A1 - Mezera, Marek A1 - Weise, Matthias A1 - Sahre, Mario A1 - Wasmuth, Karsten A1 - Hertwig, Andreas A1 - Krüger, Jörg A1 - Hodoroaba, Vasile-Dan T1 - Chemical and structural changes at the surface of titanium materials upon irradiation with near-infrared ultrashort laser pulses N2 - Due to its large strength-to-weight ratio and excellent biocompatibility, titanium materials are of paramount importance for medical applications, e.g. as implant material for protheses. In this work, the evolution of various types of laser-induced micro- and nanostructures emerging on titanium or titanium alloys upon irradiation by near-infrared ultrashort laser pulses (925 fs, 1030 nm) in air environment is studied for various laser fluence levels, effective number of pulses and at different pulse repetition rates (1 – 400 kHz). The morphologies of the processed surfaces were systematically characterized by optical and scanning electron microscopy (OM, SEM). Complementary white-light interference microscopy (WLIM) revealed the corresponding surface topographies. Chemical and structural changes were analysed through depth-profiling time-of-flight secondary ion mass spectrometry (TOF-SIMS) and X-ray diffraction (XRD) analyses. The results point towards a remarkable influence of the laser processing parameters on the surface topography, while simultaneously altering the near-surface chemistry via laser-induced oxidation effects. Consequences for medical applications are outlined. T2 - E-MRS Spring Meeting 2022 CY - Online meeting DA - 30.05.2022 KW - Laser-induced periodic surface structures (LIPSS) KW - Surface functionalization KW - ToF-SIMS KW - Chemical analysis KW - Titanium PY - 2022 AN - OPUS4-54931 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Porta-Velilla, L. A1 - Turan, N. A1 - Cubero, Á. A1 - Shao, W. A1 - Li, H. A1 - de la Fuente, G.F. A1 - Martínez, E. A1 - Larrea, Á. A1 - Castro, M. A1 - Koralay, H. A1 - Çavdar, Ş. A1 - Bonse, Jörn A1 - Angurel, L.A. T1 - Highly Regular Hexagonally-Arranged Nanostructures on Ni-W Alloy Tapes upon Irradiation with Ultrashort UV Laser Pulses N2 - Nickel tungsten alloy tapes (Ni—5 at% W, 10 mm wide, 80 µm thick, biaxially textured) used in second-generation high temperature superconductor (2G-HTS) technology were laser-processed in air with ultraviolet ps-laser pulses (355 nm wavelength, 300 ps pulse duration, 250–800 kHz pulse repetition frequency). By employing optimized surface scan-processing strategies, various laser-generated periodic surface structures were generated on the tapes. Particularly, distinct surface microstructures and nanostructures were formed. These included sub-wavelength-sized highly-regular hexagonally-arranged nano-protrusions, wavelength-sized line-grating-like laser-induced periodic surface structures (LIPSS, ripples), and larger irregular pyramidal microstructures. The induced surface morphology was characterized in depth by electron-based techniques, including scanning electron microscopy (SEM), electron back scatter diffraction (EBSD), cross-sectional transmission electron microscopy (STEM/TEM) and energy dispersive X-ray spectrometry (EDS). The in-depth EBSD crystallographic analyses indicated a significant impact of the material initial grain orientation on the type of surface nanostructure and microstructure formed upon laser irradiation. Special emphasis was laid on high-resolution material analysis of the hexagonally-arranged nano-protrusions. Their formation mechanism is discussed on the basis of the interplay between electromagnetic scattering effects followed by hydrodynamic matter re-organization after the laser exposure. The temperature stability of the hexagonally-arranged nano-protrusion was explored in post-irradiation thermal annealing experiments, in order to qualify their suitability in 2G-HTS fabrication technology with initial steps deposition temperatures in the range of 773–873 K. KW - Laser-induced periodic surface structures (LIPSS) KW - Ultrashort laser processing KW - Hexagonally-arranged nano-protrusions KW - Second-generation high temperature superconductor technology KW - Electron microscopy PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-552551 DO - https://doi.org/10.3390/nano12142380 SN - 2079-4991 VL - 12 IS - 14 SP - 1 EP - 23 PB - MDPI CY - Basel, Switzerland AN - OPUS4-55255 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Linberg, Kevin A1 - Röder, Bettina A1 - Al-Sabbagh, Dominik A1 - Emmerling, Franziska A1 - Michalchuk, Adam T1 - Controlling polymorphism in molecular cocrystals by variable temperature ball milling N2 - Mechanochemistry offers a unique opportunity to modify and manipulate crystal forms, often providing new products as compared with conventional solution methods. While promising, there is little known about how to control the solid form through mechanochemical means, demanding dedicated investigations. Using a model organic cocrystal system (isonicotinamide:glutaric acid), we here demonstrate that with mechanochemistry, polymorphism can be induced in molecular solids under conditions seemingly different to their conventional thermodynamic (thermal) transition point. Whereas Form II converts to Form I upon heating to 363 K, the same transition can be initiated under ball milling conditions at markedly lower temperatures (348 K). Our results indicate that mechanochemical techniques can help to reduce the energy barriers to solid form transitions, offering new insights into controlling polymorphic forms. Moreover, our results suggest that the nature of mechanochemical transformations could make it difficult to interpret mechanochemical solid form landscapes using conventional equilibrium-based tools. KW - Mechanochemistry KW - Polymorphism KW - TRIS PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-564728 DO - https://doi.org/10.1039/d2fd00115b SP - 1 EP - 16 PB - Royal Society of Chemistry AN - OPUS4-56472 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Linberg, Kevin A1 - Röder, Bettina A1 - Al-Sabbagh, Dominik A1 - Emmerling, Franziska A1 - Michalchuk, Adam T1 - Polymorphism in molecular cocrystals controlled by variable temperature ball milling N2 - Mechanochemistry offers a unique opportunity to modify or synthesize new crystal forms. Although the method is very promising, little is known about the mechanochemical means to control the synthesis of a solid form. Using an polymorphic organic cocrystal system, we show here that mechanochemistry can be used to obtain a polymorph transformation under the apparently conventional (thermal) transition point. T2 - Bessy User Meeting 2022 CY - Online meeting DA - 08.12.2022 KW - Mechanochemistry KW - Polymorphism KW - TRIS PY - 2022 AN - OPUS4-56473 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stawski, Tomasz A1 - Van Driessche, A. E. S. T1 - Particle-mediated origins of mesocrystalline disorder in calcium sulfate single crystals N2 - Calcium sulfate minerals are abundant in natural and engineered environments and they exist in the form of three hydrates: gypsum (CaSO4·2H2O), bassanite (CaSO4·0.5H2O), and anhydrite (CaSO4). Due to their relevance in natural and industrial processes, the formation pathways of these calcium sulfate phases from aqueous solution have been the subject of intensive research1. The state-of-the-art of the calcium sulfate formation mechanisms builds upon and goes beyond what we have come to appreciate in the astounding intricacy of other mineral formation processes from ions in aqueous solutions. The original, and rather naive, 'textbook' image of these phenomena, stemming from the adaptation of classical nucleation and growth theories, has increased in complexity due to the discovery of a variety of precursor and intermediate species2. These include solute clusters (e.g. prenucleation clusters, PNCs), liquid(-like) phases, as well as amorphous and nanocrystalline solids etc.. In this context, a number of studies have already revealed that nucleation in the CaSO4-H2O system is non-classical, where the formation of the different crystalline phases involves several steps including a common amorphous precursor1, 3, 4. In this contribution we show that the formation of the amorphous phase involves the aggregation of small primary particles into larger disordered aggregates exhibiting a "brick-in-the-wall" structure5, 6. The actual crystallization occurs by the restructuring and coalescence of the particles ("bricks") into a given calcium sulfate phase depending on the physicochemical conditions of the solution. Importantly, the rearrangement process does not continue until a (nearly-)perfect homogeneous single crystal is obtained. Instead it comes to a stop, or at least significantly slows down. Such a process thus yields a final imperfect mesocrystal, composed of smaller domains rather than a continuous crystal structure, within which the domains are separated by an amorphous (i.e. less ordered) calcium sulfate phase. Hence, the non-classical crystallization process of CaSO4 yields a final imperfect mesocrystal with an overall morphology resembling that of a single crystal, yet composed of smaller nano-domains. Importantly, these observations reveal that organic-free calcium sulfate mesocrystals grown by a particle mediated-pathway preserve in the final crystal structure a “memory” or “imprint” of their non-classical nucleation process, something that has been overlooked until now. Furthermore, the nano-scale misalignment of the structural sub-units within these crystals can propagate through the length-scales, and be expressed macroscopically as misaligned zones/domains in large single crystals (Fig. 1). Indeed, by considering large anhydrite crystals from the famous Naica Mine (“Cueva de los cristales”) we observed a suite of correlated self-similar void defects spanning multiple length-scales7 (Fig 2). These flaws, in the macroscopic crystal, stem from “seeds of imperfection” originating from a particle-mediated nucleation pathway. Hence, building a crystal could be viewed as Nature stacking blocks in a game of Tetris, whilst slowly forgetting the games core concept and failing to fill rows completely. T2 - Granada Münster Discussion Meeting (GMDM) CY - Granda, Spain DA - 30.11.2022 KW - Anhydrite KW - Mesocrystals KW - Calcium sulfate KW - Bassanite KW - Gypsum PY - 2022 AN - OPUS4-56476 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lifka, S. A1 - Harsányi, K. A1 - Baumgartner, E. A1 - Pichler, L. A1 - Baiko, D. A1 - Wasmuth, Karsten A1 - Heitz, J. A1 - Meyer, M. A1 - Joel, A.-C. A1 - Bonse, Jörn A1 - Baumgartner, W. ED - Mail, M. T1 - Laser-processed antiadhesive bionic combs for handling nanofibers inspired by nanostructures on the legs of cribellate spiders N2 - Nanofibers are drawing the attention of engineers and scientists because their large surface-to-volume ratio is favorable for applications in medicine, filter technology, textile industry, lithium-air batteries, and optical sensors. However, when transferring nanofibers to a technical product in the form of a random network of fibers, referred to as nonwoven fabric, the stickiness of the freshly produced and thus fragile nanofiber nonwoven remains a problem. This is mainly because nanofibers strongly adhere to any surface because of van der Waals forces. In nature, there are animals that are actually able to efficiently produce, process, and handle nanofibers, namely cribellate spiders. For that, the spiders use the calamistrum, a comb-like structure of modified setae on the metatarsus of the hindmost (fourth) legs, to which the 10–30 nm thick silk nanofibers do not stick due to a special fingerprint-like surface nanostructure. In this work, we present a theoretical model of the interaction of linear nanofibers with a sinusoidally corrugated surface. This model allows for a prediction of the adhesive interaction and, thus, the design of a suitable surface structure to prevent sticking of an artificially nonwoven of nanofibers. According to the theoretical prediction, a technical analogon of the nanoripples was produced by ultrashort pulse laser processing on different technically relevant metal surfaces in the form of so-called laser-induced periodic surface structures (LIPSS). Subsequently, by means of a newly established peel-off test, the adhesion of an electrospun polyamide fiber-based nonwoven was quantified on such LIPSS-covered aluminium alloy, steel, and titanium alloy samples, as well as on polished (flat) control samples as reference and, additionally, on samples with randomly rough surfaces. The latter revealed that the adhesion of electrospun nanofiber nonwoven is significantly lowered on the nanostructured surfaces compared with the polished surfaces. KW - Laser-induced periodic surface structures (LIPSS) KW - Cribellate spiders KW - Calamistrum KW - Electrospinning KW - Nanofibers PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-561799 DO - https://doi.org/10.3762/bjnano.13.105 SN - 2190-4286 VL - 13 SP - 1268 EP - 1283 PB - Beilstein-Institut zur Förderung der Chemischen Wissenschaften CY - Frankfurt, M. AN - OPUS4-56179 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Loges, A. A1 - Scholz, G. A1 - Amadeu de Sosa, Nader A1 - Jingjing, S. A1 - Emmerling, Franziska A1 - John, T. A1 - Paulus, B. A1 - Braun, T. T1 - Studies on the local structure of the F/OH site in topaz by magic angle spinning nuclear magnetic resonance and Raman spectroscopy N2 - he mutual influence of F and OH groups in neighboring sites in topaz (Al2SiO4(F,OH)2) was investigated using magic angle spinning nuclear magnetic resonance (MAS NMR) and Raman spectroscopy. The splitting of 19F and 1H NMR signals, as well as the OH Raman band, provides evidence for hydrogen bond formation within the crystal structure. Depending on whether a given OH group has another OH group or fluoride as its neighbor, two different hydrogen bond constellations may form: either OH···O···HO or F···H···O. The proton accepting oxygen was determined to be part of the SiO4 tetrahedron using 29Si MAS NMR. Comparison of the MAS NMR data between an OH-bearing and an OH-free topaz sample confirms that the 19F signal at −130 ppm stems from F− ions that take part in H···F bonds with a distance of ∼ 2.4 Å, whereas the main signal at −135 ppm belongs to fluoride ions with no immediate OH group neighbors. The Raman OH sub-band at 3644 cm−1 stems from OH groups neighboring other OH groups, whereas the sub-band at 3650 cm−1 stems from OH groups with fluoride neighbors, which are affected by H···F bridging. The integrated intensities of these two sub-bands do not conform to the expected ratios based on probabilistic calculations from the total OH concentration. This can be explained by a difference in the polarizability of the OH bond between the different hydrogen bond constellations or partial order or unmixing of F and OH, or a combination of both. This has implications for the quantitative interpretation of Raman data on OH bonds in general and their potential use as a probe for structural (dis-)order. No indication of tetrahedrally coordinated Al was found with 27Al MAS NMR, suggesting that the investigated samples likely have nearly ideal Al/Si ratios, making them potentially useful as high-density electron microprobe reference materials for Al and Si, as well as for F. KW - Topas KW - NMR KW - XRD PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-561863 DO - https://doi.org/10.5194/ejm-34-507-2022 SN - 1617-4011 VL - 34 IS - 5 SP - 507 EP - 521 PB - Copernicus Publications CY - Göttingen AN - OPUS4-56186 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Emmerling, Franziska A1 - Hoch, C. T1 - Laudatio Prof. Dr.-Ing. Caroline Röhr N2 - It is a laudatio on the ocations of Prof. Dr.-Ing. Caroline Röhrs 60th birthday. KW - Metal-oxides PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-561877 DO - https://doi.org/10.1002/zaac.202200159 SN - 0044-2313 VL - 648 IS - 10 SP - 1 EP - 2 PB - John Wiley & Sons, Ltd AN - OPUS4-56187 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmid, Thomas A1 - Hodoroaba, Vasile-Dan T1 - Correlative Analysis by Raman and other Micro & Nanospectroscopic Imaging Techniques N2 - In the present talk the basics of the Raman spectroscopy and particularly of Raman microscopy are explained. Advantages and disadvantages of the method are highlighted through selected case studies. In the second part of the lecture examples of correlative imaging with electron, X-ray, ion and optical microscopies from micro- to the nanoscale are highlighted. T2 - Charisma School on Raman Harmonisation CY - Turin, Italy DA - 19.10.2022 KW - Raman KW - Correlative Imaging KW - Microscopy KW - Hyperspectral imaging PY - 2022 UR - https://amdgroup.inrim.it/events/vamas-sc-meeting-47/program-sc47 AN - OPUS4-56094 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Baloh, P. A1 - Bauer, L. A1 - Bendová, A. A1 - Čermák, P. A1 - Fellner, K. A1 - Ghanathe, M. A1 - Hernández Alvarez, O. E. A1 - Hricov, Š. A1 - Jochum, J. K. A1 - Kotvytska, L. A1 - Kumar, S. A1 - Labh, A. A1 - Machovec, P. A1 - Pauw, Brian Richard A1 - Ramszová, K. A1 - Walz, E. A1 - Wild, P. T1 - An Exercise in Open Data: Triple Axis Data on Si single crystal N2 - Efforts are rising in opening up science by making data more transparent and more easily available, including the data reduction and evaluation procedures and code. A strong foundation for this is the F.A.I.R. principle, building on Findability, Accessibility, Interoperability, and Reuse of digital assets, complemented by the letter T for trustworthyness of the data. Here, we have used data, which was made available by the Institute Laue-Langevin and can be identified using a DOI, to follow the F.A.I.R.+T. principle in extracting, evaluating and publishing triple axis data, recorded at IN3. KW - Open data KW - Neutron diffraction KW - Analysis KW - Open science PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-562257 DO - https://doi.org/10.48550/arXiv.2010.12086 SN - 2331-8422 SP - 1 EP - 4 PB - Cornell University CY - Ithaca, NY AN - OPUS4-56225 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Iro, M. A1 - Ingerle, D. A1 - Radtke, Martin A1 - de Oliveira Guilherme Buzanich, Ana A1 - Kregsamer, P. A1 - Streli, C. T1 - Investigation of polycapillary half lenses for quantitative confocal micro-X-ray fluorescence analysis N2 - The use of polycapillary optics in confocal micro-X-ray fluorescence analysis (CMXRF) enables the destruction-free 3D investigation of the elemental composition of samples. The energy-dependent transmission properties, concerning intensity and spatial beam propagation of three polycapillary half lenses, which are vital for the quantitative interpretation of such CMXRF measurements, are investigated in a monochromatic confocal laboratory setup at the Atominstitut of TU Wien, and a synchrotron setup on the BAMline beamline at the BESSY II Synchrotron, Helmholtz-Zentrum-Berlin. The empirically established results, concerning the intensity of the transmitted beam, are compared with theoretical values calculated with the polycap software package and a newly presented analytical model for the transmission function. The resulting form of the newly modelled energy-dependent transmission function is shown to be in good agreement with Monte Carlo simulated results for the complete energy regime, as well as the empirically established results for the energy regime between 6 keV and 20 keV. An analysis of possible fabrication errors was conducted via pinhole scans showing only minor fabrication errors in two of the investigated polycapillary optics. The energy-dependent focal spot size of the primary polycapillary was investigated in the laboratory via the channel-wise evaluation of knife-edge scans. Experimental results are compared with data given by the manufacturer as well as geometric estimations for the minimal focal spot size. Again, the resulting measurement points show a trend in agreement with geometrically estimated results and manufacturer data. KW - BAMline KW - Synchrotron KW - Capillary KW - confocal PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-562430 DO - https://doi.org/10.1107/S1600577522009699 SN - 1600-5775 VL - 29 SP - 1376 EP - 1384 PB - International Union of Crystallography CY - Chester AN - OPUS4-56243 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - de O. Primo, J. A1 - Horsth, D.F. A1 - de S. Correa, J. A1 - Das, A. A1 - Bittencourt, C. A1 - Umek, P. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Radtke, Martin A1 - Yusenko, Kirill A1 - Zanetta, C. A1 - Anaissi, F.J. T1 - Synthesis and Characterization of Ag/ZnO Nanoparticles for Bacteria Disinfection in Water N2 - n this study, two green synthesis routes were used for the synthesis of Ag/ZnO nanoparticles, using cassava starch as a simple and low-cost effective fuel and Aloe vera as a reducing and stabilizing agent. The Ag/ZnO nanoparticles were characterized and used for bacterial dis- infection of lake water contaminated with Escherichia coli (E. coli). Characterization indicated the formation of a face-centered cubic structure of metallic silver nanoparticles with no insertion of Ag into the ZnO hexagonal wurtzite structure. Physicochemical and bacteriological analyses described in “Standard Methods for the Examination of Water and Wastewater” were used to evaluate the efficiency of the treatment. In comparison to pure ZnO, the synthesized Ag/ZnO nanoparticles showed high efficiencies against Escherichia coli (E. coli) and general coliforms present in the lake water. These pathogens were absent after treatment using Ag/ZnO nanoparticles. The results indicate that Ag/ZnO nanoparticles synthesized via green chemistry are a promising candidate for the treatment of wastewaters contaminated by bacteria, due to their facile preparation, low-cost synthesis,and disinfection efficiency. KW - Synchrotron KW - BAMline PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-562440 DO - https://doi.org/10.3390/nano12101764 SN - 2079-4991 VL - 12 IS - 10 SP - 1 EP - 18 PB - MDPI CY - Basel AN - OPUS4-56244 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin A1 - Cakir, Cafer Tufan T1 - Big to Small - Getting Smarter@BAMline N2 - In this talk an overview about artificial intelligence/machine learning applications @BAMline is given. In the first part, the use of neural networks for the quantification of XRF measurements and the decoding of coded-aperture measurements are shown. Then it is shown how Gaussian processes and Bayesian statistics can be used to achieve an optimal alignment of the set-up and in general for optimization of measurements. T2 - Forschungsseminar Institut für Optik und Atomare Physik TU Berlin CY - Berlin, Germany DA - 25.10.2022 KW - Artificial Inelligence KW - Machine Learning KW - Bayesian Statistics KW - Gaussian process KW - Neural network KW - BAMline KW - Synchrotron PY - 2022 AN - OPUS4-56249 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weidner, Steffen T1 - MALDI-ToF mass spectrometry for the characterization of biobased polymers suitable for depollution N2 - In this work, bio-based polymers were synthesized and designed as polymers phases for adsorption of a variety of pollutants from aqueous solutions. The obtained adsorption results showed that the integration of bio-sourced synthons generate attractive hydrophilicity, and wettability of the resulting adsorbent phase. Such polymers phases enable stronger interactions with the organic and inorganic pollutants in water. A wide variety of different bio-based polymers structures (e. g. poly(ethersulfones, poly(etherphosphines or poly(etherpyridines) with different functional groups were successfully designed in order to adapt chemical structure to different pollutants type and matrice nature. In order to characterize and to determine the correlation between polymer structures and nature of interaction with pollutants, different analytical technics (NMR, GPC, ATG, DSC, Mass spectrometry) were successfully used. Amongst them, MALDI TOF mass spectrometry plays a superior role since this technique enables the simultaneous determination of the polymer structure, polymer end groups and molecular weight. This work focusses on the characterization of synthesized polymers. The chemical structure of the repeating unit, the nature of the end groups, as well as the molecular weight, which are all important for the specific interactions of the polymer with the pollutants were clearly determined and suggestions to improve these interactions by changing the synthetic pathway could be given. T2 - 12. Journees maghreb-europe. Matériaux et Applications aux Dispositifs et Capteurs CY - Monastir, Tunisia DA - 08.11.2022 KW - MALDI TOF MS KW - Biobased polymers KW - Depollution PY - 2022 AN - OPUS4-56237 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stawski, Tomasz A1 - Van Driessche, A. T1 - Particle-mediated origins of mesocrystalline disorder in calcium sulfate single crystals N2 - Calcium sulfate minerals are abundant in natural and engineered environments and they exist in the form of three hydrates: gypsum (CaSO4·2H2O), bassanite (CaSO4·0.5H2O), and anhydrite (CaSO4). Due to their relevance in natural and industrial processes, the formation pathways of these calcium sulfate phases from aqueous solution have been the subject of intensive research1. The state-of-the-art of the calcium sulfate formation mechanisms builds upon and goes beyond what we have come to appreciate in the astounding intricacy of other mineral formation processes from ions in aqueous solutions. The original, and rather naive, 'textbook' image of these phenomena, stemming from the adaptation of classical nucleation and growth theories, has increased in complexity due to the discovery of a variety of precursor and intermediate species2. These include solute clusters (e.g. prenucleation clusters, PNCs), liquid(-like) phases, as well as amorphous and nanocrystalline solids etc.. In this context, a number of studies have already revealed that nucleation in the CaSO4-H2O system is non-classical, where the formation of the different crystalline phases involves several steps including a common amorphous precursor1, 3, 4. In this contribution we show that the formation of the amorphous phase involves the aggregation of small primary particles into larger disordered aggregates exhibiting a "brick-in-the-wall" structure5, 6. The actual crystallization occurs by the restructuring and coalescence of the particles ("bricks") into a given calcium sulfate phase depending on the physicochemical conditions of the solution. Importantly, the rearrangement process does not continue until a (nearly-)perfect homogeneous single crystal is obtained. Instead it comes to a stop, or at least significantly slows down. Such a process thus yields a final imperfect mesocrystal, composed of smaller domains rather than a continuous crystal structure, within which the domains are separated by an amorphous (i.e. less ordered) calcium sulfate phase. Hence, the non-classical crystallization process of CaSO4 yields a final imperfect mesocrystal with an overall morphology resembling that of a single crystal, yet composed of smaller nano-domains. Importantly, these observations reveal that organic-free calcium sulfate mesocrystals grown by a particle mediated-pathway preserve in the final crystal structure a “memory” or “imprint” of their non-classical nucleation process, something that has been overlooked until now. Furthermore, the nano-scale misalignment of the structural sub-units within these crystals can propagate through the length-scales, and be expressed macroscopically as misaligned zones/domains in large single crystals. Indeed, by considering large anhydrite crystals from the famous Naica Mine (“Cueva de los cristales”) we observed a suite of correlated self-similar void defects spanning multiple length-scales7. These flaws, in the macroscopic crystal, stem from “seeds of imperfection” originating from a particle-mediated nucleation pathway. Hence, building a crystal could be viewed as Nature stacking blocks in a game of Tetris, whilst slowly forgetting the games core concept and failing to fill rows completely. T2 - ECCG: European Conference on Crystal Growth 7 CY - Paris, France DA - 25.07.2022 KW - Anhydrite KW - SAXS KW - Single crystal KW - Mesocrystal PY - 2022 AN - OPUS4-56276 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stawski, Tomasz A1 - Van Dreissche, A. T1 - Particle-mediated origins of mesocrystallinity in calcium sulfate single crystals N2 - Calcium sulfate minerals are abundant in natural and engineered environments in the form of three phases: gypsum (CaSO4·2H2O), bassanite (CaSO4·0.5H2O), and anhydrite (CaSO4). Due to their relevance in natural and industrial processes, the formation pathways of these phases from aqueous solution have been the subject of intensive research, a number of studies have already revealed that nucleation in the CaSO4-H2O system is non-classical, The formation of the different crystalline phases involves several steps including a common amorphous precursor. In this contribution we show that the formation of the amorphous phase involves the aggregation of small primary particles into larger disordered aggregates exhibiting a "brick-in-the-wall" structure. The actual crystallization occurs by the restructuring and coalescence of the "bricks" into a given calcium sulfate phase depending on the physicochemical conditions of the solution. Such a process yields a final imperfect mesocrystal, composed of smaller domains rather than a continuous single crystal structure. These observations reveal that organic-free calcium sulfate mesocrystals grown by a particle mediated-pathway might preserve in the final crystal structure an “imprint” of their growth pathways. Indeed, by considering large anhydrite crystals from the famous Naica Mine we observed a suite of correlated self-similar void defects spanning multiple length-scales. These flaws, in the macroscopic crystal, stem from “seeds of imperfection” originating from an original particle-mediated growth. Hence, building a crystal could be viewed as Nature stacking blocks in a game of Tetris, whilst slowly forgetting the games core concept and failing to fill rows completely. T2 - GeoMinKöln 2022 CY - Cologne, Germany DA - 11.09.2022 KW - Anhydrite KW - Mesocrystals KW - Calcium sulfate PY - 2022 AN - OPUS4-56277 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abderrazak, H. A1 - Marestin, C. A1 - Ibtissem, J. A1 - Mercier, R. A1 - Casablanca, H. A1 - Souissi, R. A1 - Weidner, Steffen A1 - Jaffrezic, N. A1 - Chatti, Saber T1 - Synthesis of new bio based adsorbent phases N2 - Over the years, industrial and human activities and agricultural practices have caused a serious threat to human health and the environment. Indeed, it has been demonstrated that these activities are responsible for the presence of pollutants in the soil, air and water. Water is one of the most strategic issues today, as it is associated with the living world. Therefore, water pollution is becoming a universal scourge that leads to environmental degradation, decrease of water quality and threatens public health. Water pollution is mainly due to the discharge of certain harmful chemical compounds that are not very or not at all biodegradable (phenolic compounds, heavy metals, hydrocarbons, dyes, pesticides, etc.) by various industries: chemical, pharmaceutical, textile, food processing, etc. The impact of these industrial effluents on fauna and flora is very harmful. A sensitization of the socio-economic actors and the public, accompanied by a severe regulation in relation to the discharges, would contribute to fight against this drift, but also, by the development of effective methods allowing to remove these pollutants, not only in an analytical purpose but also of depollution. Thus and within the framework of the preservation of an environment with regard to any anthropogenic activity, our research topic relates to the use of original biosourced polymeric phases for the extraction of the organic compounds and the heavy metals in aqueous mediums. Therefore, we have proceeded to the synthesis and characterization of a large variety of monomers, polymers and cross-linked materials. These products, partially derived from biomass, contain various functional groups with the ability to interact with chemical components without discriminating effect. The developed polymer phases have been successfully used for the adsorption of some organic pollutants and heavy metals in synthetic aqueous solutions. T2 - 12. Journees maghreb-europe. Matériaux et Applications aux Dispositifs et Capteurs CY - Monastir, Tunisia DA - 08.11.2022 KW - Organic-inorganic adsorbents KW - Semi-Interpenetrating Network KW - Poly(ether-sulfone) KW - Reversible adsorption. PY - 2022 AN - OPUS4-56286 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Brirmi, N. A1 - Mercier, R. A1 - Marestin, C. A1 - Weidner, Steffen A1 - Casablanca, H. A1 - Jaffrezic, N. A1 - Ben Romdahne, H. A1 - Chatti, Saber T1 - Effect of the pendant groups on the biobased polymers obtained by click chemistry suitable for the removal of phenolic compounds from water N2 - Phenolic compounds constitute a widespread and important class of water pollutants that should be efficiently removed from wastewater because of their toxicity even at low concentrations. They are indeed discharged in the liquid effluents from various factories: chemical, petrochemical, paper, wood, metallurgy and cocking plants 1. Phenols are also found in the waste waters of agroindustrial processes like the olive oil mills, tomato processing and wine distilleries 2,3. These contaminants cause several health problems for humans and aquatic organisms 4. Therefore, numerous studies on the removal of polyphenols from wastewaters have been conducted and many techniques have been used. Among them, adsorption is considered to be the best effective and low cost method. In this context, we have focused our efforts on optimizing adsorption process by development of novel, low-cost adsorbents derived from biobased byproducts with high adsorptive capacity. The main aim of this study is to synthesize triazole-based poly(ether-pyridine)s as new synthetic adsorbent phases for the extraction of phenolic compounds from aqueous solutions. For this purpose, new fluoromonomers containing 1,2,3-triazole units were prepared by the Cu(I)-catalyzed 1,3-dipolar cycloaddition reaction and then used for the elaboration of novel poly(ether-pyridine-triazole)s (PEPTs) by direct polycondensation with isosorbide and bisphenol A. Chemical structure of fluorinated pyridinic monomers as well as resulting polymers was confirmed by 1H and 19F NMR spectroscopic methods. The thermal behaviour of the obtained PEPTs was characterized using differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). Their uptake performance to eliminate organic compounds was determined using High Performance Liquid Chromatography (HPLC). T2 - 12. Journees maghreb-europe. Matériaux et Applications aux Dispositifs et Capteurs CY - Monastir, Tunisia DA - 08.11.2022 KW - Biobased polymers KW - Phenolic compounds KW - 1,2,3-triazole PY - 2022 AN - OPUS4-56287 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin A1 - Cakir, Cafer Tufan A1 - de Oliveira Guilherme Buzanich, Ana T1 - Getting more efficient – The use of Bayesian optimization and Gaussian processes at the BAMline N2 - For more than 20 years, BAM is operating the BAMline at the synchrotron BESSY II in Berlin Adlershof. During this time, the complexity of the setup and the amount of data generated have multiplied. To increase the effectiveness and in preparation for BESSY III, algorithms from the field of machine learning are increasingly used. In this paper, several examples in the areas of beamline alignment and measurement time optimization based on Bayesian optimization (BO) with Gaussian processes (GP) are presented. BO is a method for finding the global optimum of a function using a probabilistic model represented by a GP. The advantage of this method is that it can handle high-dimensional problems, does not depend on the initial estimate, and also provides uncertainty estimates. After a short introduction to BO and GP, the first example is the automatic alignment of our double multilayer monochromator (DMM). To achieve optimal performance, up to three linear and two angular motor positions have to be optimized. To achieve this with a grid scan, at least 100^5 measurement points would be required. Assuming that all positions can be aligned independently, 100*5 points are still necessary. We show that with BO and GP less than 100 points are sufficient to achieve equal or better results. The second example is the optimization of measurement time in XRF scanning. Here we will show the advantage of the BO GP approach over point-by-point scanning. As can be seen in Fig. 1, the number of points required and thus the measurement time can be reduced by a factor of 50, while the loss in image quality is acceptable. The advantages and limitations of this approach will be discussed. T2 - European Conference on X-ray Spectrometry 2022 CY - Bruges, Belgium DA - 26.06.2022 KW - Artificial Inelligence KW - Machine Learning KW - Bayesian Statistics KW - Gaussian process KW - Neural network KW - BAMline KW - Synchrotron PY - 2022 AN - OPUS4-56251 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - From Egypt to Hiddensee – Analysis of Gold with Synchrotron Radiation IV N2 - Gold is one of the seven metals already known in antiquity and was used from time immemorial as a medium of exchange and for the production of jewelry because of its luster and rarity. In addition, it is easy to work and largely resistant to chemical influences. Investigations of gold using synchrotron radiation excited X-ray fluorescence analysis are non-destructive and provide information about the chemical elements present in the sample under investigation. The investigations presented here at BAMline focus on questions such as the origin, manufacturing process, and association of gold findings. The different questions are explained by a number of examples ranging from the Viking treasure from Hiddensee to the Nebra Sky Disk and finds from Egypt. The find from Bernstorf is discussed in detail. A Bayesian treatment of the authenticity is shown. T2 - Ringvorlesung Einführung in die Archäometrie CY - Berlin, Germany DA - 04.11.2022 KW - Synchrotron KW - BAMline KW - Bayesian Statistics KW - Gold KW - Röntgenfluoreszenz PY - 2022 AN - OPUS4-56252 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - News from the BAMline N2 - A presentation of recent measurements at the BAMline with focus on AI and ML applications T2 - Seminar: Strahlenphysikalische Anwendungen in Technik und Medizin CY - Vienna, Austria DA - 18.05.2022 KW - Synchrotron KW - BAMline KW - Bayesian Statistics KW - Gold KW - X-ray fluorescence PY - 2022 AN - OPUS4-56253 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Olbrich, Adelina-Elisa A1 - An Stepec, Biwen Annie A1 - Wurzler, Nina A1 - Terol, E. C. A1 - Koerdt, Andrea A1 - Meermann, Björn T1 - Beyond corrosion: Development of a single cell-ICP-ToF-MS method to uncover the process of microbiologically influenced corrosion N2 - The development of the microbiologically influenced corrosion ( MIC ) -specific inductively coupled plasma-time of flight-mass spectrometry ( ICP-ToF-MS ) analytical method presented here, in combination with the investigation of steel-MIC interactions, contributes significantly to progress in instrumental MIC analysis. For this, a MIC-specific staining procedure was developed, which ensures the analysis of intact cells. It allows the analysis of archaea at a single cell level, which is extremely scarce compared to other well-characterized organisms. The detection method revealed elemental selectivity for the corrosive methanogenic strain Methanobacterium -affiliated IM1. Hence, the possible uptake of individual elements from different steel samples was investigated and results showed the cells responded at a single-cell level to the different types of supplemented elements and displayed the abilities to uptake chromium, vanadium, titanium, cobalt, and molybdenum from solid metal surfaces. The methods developed and information obtained will be used in the future to elucidate underlying mechanisms, compliment well-developed methods, such as SEM-EDS, and develop novel material protection concepts. KW - Single cell KW - Microbiological influenced corrosion MIC KW - Sc-ICP-ToF-MS KW - Method development KW - Ir DNA staining approach KW - Carbon steel corrosion PY - 2022 DO - https://doi.org/10.1093/mtomcs/mfac083 SN - 1756-591X VL - 14 IS - 11 SP - 1 EP - 15 PB - Oxford University Press CY - Oxford AN - OPUS4-56254 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin A1 - Cakir, Cafer Tufan A1 - de Oliveira Guilherme Buzanich, Ana T1 - Getting more efficient – The use of Bayesian optimization and Gaussian processes at the BAMline N2 - For more than 20 years, BAM is operating the BAMline at the synchrotron BESSY II in Berlin Adlershof. During this time, the complexity of the setup and the amount of data generated have multiplied. To increase the effectiveness and in preparation for BESSY III, algorithms from the field of machine learning are increasingly used. After a short introduction to BO and GP, the first example is the automatic alignment of our double multilayer monochromator (DMM). The second example is the optimization of measurement time in XRF scanning. T2 - SNI2022 conference CY - Berlin, Germany DA - 05.09.2022 KW - Artificial Inelligence KW - Machine Learning KW - Bayesian Statistics KW - Gaussian process KW - X-ray fluorescence KW - BAMline PY - 2022 AN - OPUS4-56255 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - de Oliveira Guilherme Buzanich, Ana A1 - Michalchuk, Adam A1 - Cakir, Cafer Tufan A1 - Haider, M. B. A1 - Yusenko, Kirill A1 - Radtke, Martin A1 - Reinholz, U. A1 - Emmerling, Franziska T1 - Time resolved in situ monitoring of mechanochemical transformations by X-ray spectroscopy (XAS) N2 - Mechanochemical reactions promise a new direction for environmentally benign preparation of materials, and has been dubbed by IUPAC as one of the 10 chemical innovations that will change our world. Despite this significant promise, very little is known about the mechanisms that drive mechanochemical transformations, posing significant barriers to realizing their full potential. To this end, there is growing need to follow mechanochemical reactions in situ and in real time. We here describe advances in the development and application of XAS methods to monitor material synthesis in real time under mechanochemical conditions. We demonstrate the generality of our approaches by describing mechanochemical syntheses of materials by both vibratory ball milling and by Resonant Acoustic Mixing (RAM), where a time resolution of 1 second is for a whole XAS spectrum was achieved. Moreover, we describe how spectroscopic methods can be coupled to diffraction-based approaches, thereby providing new dimensions in understanding mechanochemical synthesis. T2 - AfLS3 CY - Online meeting DA - 14.11.2021 KW - Dipsersive XAS KW - Mechanochemistry KW - Time-resolved KW - In situ PY - 2021 AN - OPUS4-56256 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - de Oliveira Guilherme Buzanich, Ana A1 - Michalchuk, Adam A1 - Cakir, Cafer Tufan A1 - Yusenko, Kirill A1 - Radtke, Martin A1 - Reinholz, U. A1 - Emmerling, Franziska T1 - Time resolved in situ monitoring of mechanochemical transformations by X-ray spectroscopy (XAS) N2 - Mechanochemical reactions promise a new direction for environmentally benign preparation of materials, and has been dubbed by IUPAC as one of the 10 chemical innovations that will change our world. Despite this significant promise, very little is known about the mechanisms that drive mechanochemical transformations, posing significant barriers to realizing their full potential. To this end, there is growing need to follow mechanochemical reactions in situ and in real time. We here describe advances in the development and application of XAS methods to monitor material synthesis in real time under mechanochemical conditions. We demonstrate the generality of our approaches by describing mechanochemical syntheses of materials by both vibratory ball milling and by Resonant Acoustic Mixing (RAM), where a time resolution of 1 second is for a whole XAS spectrum was achieved. Moreover, we describe how spectroscopic methods can be coupled to diffraction-based approaches, thereby providing new dimensions in understanding mechanochemical synthesis. T2 - Denver X-ray Conference: DXC 2021 CY - Online meeting DA - 02.08.2021 KW - Dispersive XAS KW - Mechanochemistry KW - Time resolved KW - In situ PY - 2021 AN - OPUS4-56257 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - de Oliveira Guilherme Buzanich, Ana T1 - Time resolved in situ monitoring of mechanochemical transformations by X-ray absorption spectroscopy (XAS) N2 - Mechanochemical reactions promise a new direction for environmentally benign preparation of materials, and has been dubbed by IUPAC as one of the 10 chemical innovations that will change our world. Despite this significant promise, very little is known about the mechanisms that drive mechanochemical transformations, posing significant barriers to realizing their full potential. To this end, there is growing need to follow mechanochemical reactions in situ and in real time. We here describe advances in the development and application of XAS methods to monitor material synthesis in real time under mechanochemical conditions. We demonstrate the generality of our approaches by describing mechanochemical syntheses of materials by both vibratory ball milling and by Resonant Acoustic Mixing (RAM), where a time resolution of 1 second is for a whole XAS spectrum was achieved. Moreover, we describe how spectroscopic methods can be coupled to diffraction-based approaches, thereby providing new dimensions in understanding mechanochemical synthesis. T2 - European Conference on X-ray Spectrometry 2022 CY - Bruges, Belgium DA - 27.06.2022 KW - XAS KW - Mechanochemictry KW - Time resolved KW - In situ PY - 2022 AN - OPUS4-56258 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - de Oliveira Guilherme Buzanich, Ana T1 - Time resolved in situ monitoring of mechanochemical transformations by X-ray absorption spectroscopy (XAS) N2 - Mechanochemical reactions promise a new direction for environmentally benign preparation of materials, and has been dubbed by IUPAC as one of the 10 chemical innovations that will change our world. Despite this significant promise, very little is known about the mechanisms that drive mechanochemical transformations, posing significant barriers to realizing their full potential. To this end, there is growing need to follow mechanochemical reactions in situ and in real time. We here describe advances in the development and application of XAS methods to monitor material synthesis in real time under mechanochemical conditions. We demonstrate the generality of our approaches by describing mechanochemical syntheses of materials by both vibratory ball milling and by Resonant Acoustic Mixing (RAM), where a time resolution of 1 second is for a whole XAS spectrum was achieved. Moreover, we describe how spectroscopic methods can be coupled to diffraction-based approaches, thereby providing new dimensions in understanding mechanochemical synthesis. T2 - Advances X ray Analytics Seminar at TU Berlin CY - Berlin, Germany DA - 14.06.2022 KW - XAS KW - Mechanochemistry KW - Time resolved KW - In situ PY - 2022 AN - OPUS4-56259 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Heilmann, Maria T1 - Nanoparticle Populations N2 - Two new projects P15 Measurement of particle size and shape distribution of bipyramidal titania including deposition from liquid suspension and P16 Measurement of (relative) number concentration of bimodal silica nanoparticles including deposition from liquid suspension have been started at VAMAS/TWA 34 under the lead of BAM. First results are presented and discussed. T2 - Versailles Project on Advanced Materials and Standards (VAMAS) 47th Steering Committee Meeting CY - Turin, Italy DA - 18.10.2022 KW - VAMAS KW - Nanoparticles KW - Inter-laboratory comparison KW - Particle size distribution KW - Nanoparticle concentration PY - 2022 AN - OPUS4-56196 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Cakir, Cafer Tufan A1 - de Oliveira Guilherme Buzanich, Ana A1 - Reinholz, Uwe A1 - Emmerling, Franziska A1 - Streli, Christina A1 - Radtke, Martin T1 - High Speed for High Entropy Materials N2 - Time is the most valuable parameter in synchrotron experiments. This is costly and some of the experiments suffer from low efficiency due to low counting statistics. With today's high processing power long experiments are run in a shorter time and increase efficiency. With optimization algorithms time in "counting-hungry" experiments reduced by factor of 10. Our project is to develop a new method to analyze the chemical properties of complex materials non-destructively and efficiently, such as high entropy materials subjected to corrosion processes. A better understanding of the corrosion process will help to develop corrosion-resistant materials and reduce the cost of corrosion damage, which averages around 2.5 trillion USD annually. T2 - Berlin Science Week CY - Berlin, Germany DA - 01.11.2022 KW - GEXRF KW - High entropy alloys KW - XANES KW - High entropy materials KW - Grazing exit KW - XAS KW - Optimization PY - 2022 AN - OPUS4-56269 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Cakir, Cafer Tufan A1 - de Oliveira Guilherme Buzanich, Ana A1 - Reinholz, Uwe A1 - Emmerling, Franziska A1 - Streli, Christina A1 - Radtke, Martin T1 - Optimization of Depth Resolved X-Ray Absorption Spectroscopy in Grazing Emission Mode for Characterizing Compositionally Complex Alloys N2 - The components that are used in structural and in high temperature applications generally face significant challenges with respect to oxidation behaviours and metalworking processes. In most of the cases, harsh environmental conditions lead materials to degrade due to corrosion. To thoroughly investigate the corrosion processes and to determine oxidation states of metal components within the reaction products, we need special analytical tools. Grazing exit X-ray fluorescence (GEXRF) offers a non-destructive way to collect this information in sub-micrometre depth range. In order to obtain structural information, such as regarding oxidation states or atomic/molecular geometric arrangement, the GEXRF approach can also be combined with the X-ray absorption spectroscopy (XAS) method. The position and energy sensitive detector, with 264x264 pixel detector area, provides information regarding the signal emitted from the sample as a function of the emission angle and thus allows depth-sensitive analysis. Furthermore, the data collected from samples of an incidence energy which can be controlled with a resolution of 0.5 eV provides XANES data to determine oxidation states. We address the feasibility of our setup and provide a new optimization procedure (Bayesian Optimization and Gaussian Regression) to decrease measuring time. The results settle on a conceptual study on a reference sample (Cr-Oxide layer (300nm) on Cr layer (500nm) on Si wafer). T2 - XAFS 2022, The 19th International XAFS Conference CY - Sydney, Australia DA - 10.07.2022 KW - GEXRF KW - High entropy alloys KW - XANES KW - Grazing exit KW - High entropy materials KW - Optimization KW - XAS PY - 2022 AN - OPUS4-56270 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Cakir, Cafer Tufan A1 - de Oliveira Guilherme Buzanich, Ana A1 - Reinholz, Uwe A1 - Emmerling, Franziska A1 - Streli, Christina A1 - Radtke, Martin T1 - Scanning-Free Grazing Exit XANES Analysis of Stratified Samples and the Optimization of the Data Collection Process N2 - The components that are used in structural and in high temperature applications generally face significant challenges with respect to oxidation behaviours and metalworking processes. In most of the cases, harsh environmental conditions lead materials to degrade due to corrosion. To thoroughly investigate the corrosion processes and to determine oxidation states of metal components within the reaction products, we need special analytical tools. Grazing exit X-ray fluorescence (GEXRF) offers a non-destructive way to collect this information in sub-micrometre depth range. In order to obtain structural information, such as regarding oxidation states or atomic/molecular geometric arrangement, the GEXRF approach can also be combined with the X-ray absorption spectroscopy (XAS) method. The position and energy sensitive detector, with 264x264 pixel detector area, provides information regarding the signal emitted from the sample as a function of the emission angle and thus allows depth-sensitive analysis. Furthermore, the data collected from samples of an incidence energy which can be controlled with a resolution of 0.5 eV provides XANES data to determine oxidation states. We address the feasibility of our setup and provide a new optimization procedure (Bayesian Optimization and Gaussian Regression) to decrease measuring time. The results settle on a conceptual study on a reference sample (Cr-Oxide layer (300nm) on Cr layer (500nm) on Si wafer). T2 - Denver X-Ray Conference DXC 2022 CY - Washington D.C., USA DA - 07.08.2022 KW - GEXRF KW - High entropy alloys KW - High entropy materials KW - Optimization KW - XANES KW - Grazing exit KW - XAS PY - 2022 AN - OPUS4-56271 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Cakir, Cafer Tufan A1 - de Oliveira Guilherme Buzanich, Ana A1 - Reinholz, Uwe A1 - Emmerling, Franziska A1 - Streli, C. A1 - Radtke, Martin T1 - Bayesian optimization for depth resolved analysis of complex alloys with grazing exit XANES N2 - Compositionally complex alloys (CCAs) are a new class of alloys containing at least 5 elements with concentrations between 5 and 35 atomic percent. Due to their adjustable composition, which enables modifications of mechanical properties (such as hardness, strength and ductility etc) and their stability at high temperatures, CCAs have been the focus of various studies [1,2]. Especially the corrosion behavior of CCAs has been a wide research interest. However, there are only few studies that deals with the degradation process on such materials, which is highly relevant for the safety aspect for future component design. To thoroughly investigate the corrosion processes and to determine oxidation states of metal components within the reaction products, we need special analytical tools. Since the grazing exit X-ray fluorescence (GEXRF) offers a non-destructive way to collect notable information regarding the high temperature oxidation, we consider it as a useful method to investigate how CCAs behave in corrosive environments. The main idea of grazing geometry is to enhance the fluorescence signal of the surface. This enables highly sensitive surface analyses of thin protective film on surface in sub-micrometer scale [3]. When compared to a conventional CCD-based camera, the advantage and most important feature of the detector system (Color X-Ray Camera (CXC)) is that each pixel is an energy sensitive detector. The position and area sensitive detector, with 264x264 pixel detector area, provides information regarding the signal emitted from the sample as a function of the emission angle and thus allows depth-sensitive analysis. Furthermore, the data collected from samples of an incidence energy which can be controlled with a resolution of 0.5 eV provides XANES data to determine oxidation states. In this contribution, we address the feasibility of our setup and new optimization procedure (Bayesian Optimization and Gaussian Regression). The results of a conceptual study regarding layer properties of the reference sample (Cr-Oxide layer (300nm) on Cr layer (500nm) on Si wafer) and CrCoNi (Cr-Oxide (>1µm) layer on CrCoNi substrate) medium entropy alloy. T2 - European Conference on X-ray Spectrometry. EXRS 2022 CY - Bruges, Belgium DA - 26.06.2022 KW - GEXRF KW - High entropy alloys KW - XANES KW - Grazing exit KW - High entropy materials KW - XAS KW - Optimization PY - 2022 AN - OPUS4-56272 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Madkour, Sherif A. A1 - Gawek, Marcel A1 - Penner, P. A1 - Paneff, F. A1 - Zhang, X. A1 - Gölzhäuser, A. A1 - Schönhals, Andreas T1 - Can Polymers be Irreversibly Adsorbed on Carbon Nanomembranes? A Combined XPS, AFM, and Broadband Dielectric Spectroscopy Study N2 - Carbon nanomembranes are synthetic two-dimensional sheets with nanometer thickness, macroscopic lateral dimensions, and high structural homogeneity. They have great application potential in various branches of nanotechnology. Because of their full carbon structure, it is not clear whether macromolecules like poly(methyl methacrylate) (PMMA) can be irreversibly adsorbed on their surface. Here, irreversible adsorption means that the polymer chains cannot be removed by a leaching process, which is assumed in technological transfer processes. However, if polar defects are present on the carbon nanomembranes (CNMs), it may occur that polymers can be irreversibly adsorbed. To address this question, PMMA was spin-coated on top of CNMs, annealed for a specific time at different temperatures, and then tried to be removed by a acetone treatment in a leaching approach. The samples were investigated in detail by atomic force microscopy, X-ray photoelectron spectroscopy, and broadband dielectric spectroscopy, where the latter method has been applied to CNMs for the first time. Unambiguously, it was shown that PMMA can be adsorbed on the surface of CNMs after annealing the sample above the glasstransition temperature of PMMA. The general occurrence of polar defects on the surface of CNMs and the adsorption of polymers open opportunities for advanced innovative hybrid materials combining the properties of the CNM with those of the polymer. KW - Carbon Nanomembranes KW - Irreversible adsorption KW - Broadband dielectric spectroscopy KW - XPS spctroscopy KW - Atomic force microscopy PY - 2022 DO - https://doi.org/10.1021/acsapm.2c01320 SN - 2637-6105 VL - 4 IS - 11 SP - 8377 EP - 8385 PB - ACS AN - OPUS4-56067 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - del Giorgio, Elena A1 - Kumari, P. A1 - Lymer, K. A1 - Connell, S. A1 - Zhang, S. A1 - Hodoroaba, Vasile-Dan A1 - Pikramenou, Z. T1 - Visible and NIR emissive lanthanide(III) surfaces for new luminescent materials N2 - Luminescent lanthanides(III) offer exceptional optical properties that can overcome issues often encountered with other fluorophores (e.g. organic dyes). Their long lifetimes up to milliseconds, low photobleaching and sharp and characteristic emission peaks make the lanthanides extremely valuable for the development of advanced luminescent materials. Previous work on Ru(II) and Ir(III) gold surfaces further highlights the potential of employing the luminescence of metal complexes for the fabrication of sensing platforms and devices. Here, we incorporate visible and NIR-emitting lanthanide(III) complexes Ln2L3 (Ln = Eu(III), Nd(III), Yb(III)) to gold and plasmonic surfaces, translating the unique optical properties of the lanthanides(III) to practical devices. The Ln2L3 complexes are deposited on the surfaces with different methods, ranging from polymer aided physisorption to the covalent attachment on the gold surface. Furthermore, we exploit the high sensitivity to the coordination environment of lanthanides(III) to design and prepare a sensing platform. T2 - 17th Conference on Methods and Applications in Fluorescence (MAF 2022) CY - Göteborg, Sweden DA - 11.09.2022 KW - Luminescent materials KW - Lanthanide(III) KW - Surface morphology KW - AFM KW - SEM/EDS PY - 2022 UR - https://maf2022.com/ AN - OPUS4-56126 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - George, Janine T1 - Mit Hilfe künstlicher Intelligenz neue Materialien finden N2 - In diesem Vortrag für Schüler*innen, die an der nationalen Auswahl der internationalen Chemieolympiade teilnehmen, stellte ich meinen akademischen Werdegang und das Fach Materialinformatik und die Forschung in diesem Bereich vor. T2 - Landesseminar zur Internationalen Chemieolympiade in Berlin-Brandenburg CY - Berlin, Germany DA - 30.10.2022 KW - Materialinformatik KW - Automatisierung KW - Computerchemie PY - 2022 AN - OPUS4-56128 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ermilova, Elena A1 - Weise, Matthias A1 - Hertwig, Andreas T1 - Hybrid optical measurement technique for detection of defects in epitaxially grown 4H-SiC layers N2 - Recent developments in power electronics require the use of new wide bandgap compound semiconductor. We demonstrate the use of the ellipsometry and white light interference microscopy to detect defects in epitaxially grown SiC layers on SiC substrates. Such hybrid optical metrology methods can be used to better understand the mechanism of the development of the defects as well as their effects on the material´s optoelectronic properties. T2 - EOS Annual Meeting (EOSAM 2022) CY - Porto, Portugal DA - 12.09.2022 KW - Imaging ellipsometry KW - White light interference microscopy KW - Wide bandgap compound semiconductor KW - Epitaxially grown 4H-SiC layers PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-561113 DO - https://doi.org/10.1051/epjconf/202226610001 VL - 266 SP - 1 EP - 2 AN - OPUS4-56111 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Naik, Aakash Ashok A1 - George, Janine T1 - New descriptors for materials properties based on bonding indicators N2 - Includes a summary of the Ph.D. project that deals with generating a database populated with materials bonding properties and how we intend to gain deeper insights into material properties through this research. T2 - SALSA 2022 CY - Berlin, Germany DA - 15.09.2022 KW - Bonding analysis KW - Automation KW - Materials Informatics KW - Computational Chemistry PY - 2022 AN - OPUS4-56142 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Quantitative Microstructural Analysis - VAMAS TWA 37 & Liaison with ISO/TC 202 Microbeam Analysis N2 - The progress in activities on Microbeam Analysis under VAMAS/TWA 37 is reviewed. Particularly the liaison with the new projects within the ISO technical committee TC 202 is presented and discussed with respect to the possibility of identifying and launching related VAMAS projects. The recently started project FIB sample processing for TEM is highlighted. Need of more promotion for the engagement of more participants from industry and academia at national, European and international level is highlighted. Also, the competition with the other technical working areas (on 'nano' or materials-related) is critically discussed. Further, a short overview of the VAMAS areas of activities is given where Germany is involved. Planed regional VAMAS Workshops in Germany in 2023 are announced. T2 - Versailles Project on Advanced Materials and Standards (VAMAS) 47th Steering Committee Meeting CY - Torino, Italy DA - 18.10.2022 KW - VAMAS KW - Microbeam analysis KW - FIB KW - TEM KW - Sample preparation KW - EBSD PY - 2022 UR - https://amdgroup.inrim.it/events/vamas-sc-meeting-47 AN - OPUS4-56146 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Pauw, Brian Richard A1 - Smales, Glen Jacob T1 - X-ray scattering Datasets of gold and silver nanoparticle composites, relating to the publication "Gold and silver dichroic nanocomposite in the quest for 3D printing the Lycurgus cup" N2 - Wide-range X-ray scattering datasets and analyses for all samples described in the 2020 publication "Gold and silver dichroic nanocomposite in the quest for 3D printing the Lycurgus cup". These datasets are composed by combining multiple small-angle x-ray scattering and wide-angle x-ray scattering curves into a single dataset. They have been analyzed using McSAS to extract polydispersities and volume fractions. They have been collected using the MOUSE project (instrument and methodology). KW - X-ray scattering KW - MOUSE KW - Saxs KW - Waxs KW - Analyses KW - Datasets PY - 2022 DO - https://doi.org/10.5281/zenodo.7193859 PB - Zenodo CY - Geneva AN - OPUS4-55979 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - George, Janine T1 - Data-driven chemical understanding with geometrical and quantum-chemical bonding analysis N2 - Chemical bonding and coordination environments are crucial descriptors of material properties. They have previously been applied to creating chemical design guidelines and chemical heuristics. They are currently being used as features in machine learning more and more frequently. I will discuss implementations and algorithms (ChemEnv and LobsterEnv) for identifying these coordination environments based on geometrical characteristics and chemical bond quantum chemical analysis. I'll demonstrate how these techniques helped in testing chemical heuristics like the Pauling rule and thereby improved our understanding of chemistry. I'll also show how these tools can be used to create new design guidelines and a new understanding of chemistry. To use quantum-chemical bonding analysis on a large-scale and for machine-learning approaches, fully automatic workflows and analysis tools have been developed. After presenting the capabilities of these tools, I will also point out how these developments relate to the general trend towards automation in the field of density functional based materials science. T2 - ICAMS Interdisciplinary Centre for Advanced Materials Simulation Seminar Series CY - Online meeting DA - 24.11.2022 KW - Automation KW - High-throughput KW - Machine learning KW - Materials informatics KW - Bonding Analysis PY - 2022 AN - OPUS4-56417 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - George, Janine T1 - Automation and workflows incomputational materials science N2 - This talk introduced the audience to automation and workflows in the field of computational materials science. The audience were the members of the FONDA Sonderforschungsbereich at HU Berlin T2 - FONDA Seminar Series CY - Berlin, Germany DA - 10.10.2022 KW - Automation KW - Workflows KW - Materials Informatics PY - 2022 AN - OPUS4-56419 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Karafiludis, Stephanos A1 - Kochovski, Z. A1 - Retzmann, Anika A1 - Scoppola, E. A1 - Emmerling, Franziska A1 - Stawski, Tomasz T1 - How do transition metal phosphates crystallise? N2 - Industrial and agricultural waste streams (waste waters, sludges, tailings etc.), which contain high concentrations of NH4+, PO43- and transition metals, are environmentally harmful due to their toxic pollutants. At the same time, phosphorus and selective transition metals such as Cobalt could be potentially depleted as a critical raw material due to the high demand and rapidly declining natural ore deposits. Therefore, due to simultaneous scarcity and abundance, the phosphorus and 3d metal recovery from agricultural, industrial, mining, or urban wastewaters have been an important factor in sustaining our global consumption and preservation of the natural environment. Typically, separate pathways have been considered to extract hazardous substances such as transition metals or phosphate, independently from each other. Here, we investigate the crystallization of transition metal phosphate (TMP) compounds (NH4MPO4∙6H2O, M3(PO4)2∙8H2O with M = Ni2+, Co2+, NixCo1-x2+ M-struvite and M-phosphate octahydrate) out of aqueous solutions, which allow for P, ammonia and metal co-precipitation. The precipitation of these compounds from industrial and agricultural waste waters has high potential as a P- and 3d metal recovery route. For this purpose, a detailed understanding of the crystallization process beginning from combination of solved ions and ending in a final crystalline product is required. Through adjusting the reaction conditions, the stability, crystallite size and morphology of the as-obtained TMPs could be controlled. Detailed investigations of the precipitation process in time using ex- and in-situ techniques provided new insights into their non-classical crystallization mechanism/crystal engineering of these materials. These TMPs involve transitional colloidal nanophases during the crystallization process. Over time, their complex amorphous framework changes significantly resulting simultaneously in an agglomeration and densification of the compound. After extended reaction times these colloidal nanophases condensed to a final crystal. However, the reaction kinetics of the formation of a final crystalline product and the lifetime of these intermediate phases vary significantly depending on the metal cation involved in the precipitation process. Ni-struvite is stable in a wide reactant concentration range and at different metal/phosphorus (M/P)-ratios, whereas Co tends to form Co-struvite and/or Co-phosphate octahydrate depending on the (M/P)-ratio. The mixed NixCo1-x system shows a significantly different crystallization behavior and reaction kinetics of the precipitation compared to the pure endmembers. The observed various degree of stability could be linked to the octahedral metal coordination environment in these compounds. The achieved level of control over the precipitates, is highly desirable for 3d- and P-recovery methods. Under this paradigm, the crystals can be potentially upcycled as precursor materials for (electro)catalytical applications. T2 - Granada Münster Discussion Meeting (GMDM) CY - Granada, Spain DA - 30.11.2022 KW - Struvite KW - Transition metal KW - Phosphates KW - Amorphous phases KW - Non-classical crystallization PY - 2022 AN - OPUS4-56478 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Karafiludis, Stephanos A1 - Kochovski, Z. A1 - Scoppola, E. A1 - Emmerling, Franziska A1 - Stawski, Tomasz T1 - Crystallization study of transition metal phosphates: a new example for non-classical crystallization theory N2 - Industrial and agricultural waste streams (waste waters, sludges, tailings etc.), which contain high concentrations of NH4+, PO43- and transition metals, are environmentally harmful due to their toxic pollutants. At the same time, phosphorus and selective transition metals such as Cobalt could be potentially depleted as a critical raw material due to the high demand and rapidly declining natural ore deposits. Therefore, due to simultaneous scarcity and abundance, the phosphorus and 3d metal recovery from agricultural, industrial, mining, or urban wastewaters have been an important factor in sustaining our global consumption and preservation of the natural environment. Typically, separate pathways have been considered to extract hazardous substances such as transition metals or phosphate, independently from each other. Here, we report the synthesis routes for transition metal phosphate (TMP) compounds (M3(PO4)2∙8H2O, NH4MPO4∙6H2O, M = Ni2+, Co2+, NixCo1-x2+ M-struvite and M-phosphate octahydrate), which allow for P, ammonia and metal co-precipitation. The precipitation of these compounds from industrial and agricultural waste waters could be a promising P-recovery route. Through adjusting the reaction conditions, the stability, crystallite size and morphology of the as-obtained TMP could be controlled. Detailed investigations of the precipitation process using ex- and in-situ techniques provided new insights into their non-classical crystallization mechanism/crystal engineering of these materials. These TMPs involve transitional colloidal nanophases which subsequently aggregate and condense to final crystals after extended reaction times. However, the reaction kinetics of the formation of a final crystalline product vary significantly depending on the metal cation involved in the precipitation process. Ni-struvite is stable in a wide reactant concentration range and at different metal/phosphorus (M/P)-ratios, whereas Co tends to form Co-struvite and/or Co-phosphate octahydrate depending on the (M/P)-ratio. The mixed NixCo1-x system shows a significantly different crystallization behavior and reaction kinetics of the precipitation compared to the pure endmembers. The observed various degree of stability could be linked to the octahedral metal coordination environment in these compounds. The achieved level of control over the precipitates, is highly desirable for 3d- and P-recovery methods. Under this paradigm, the crystals can be potentially upcycled as precursor materials for (electro)catalytical applications. T2 - Adlershofer Forschungsforum 2022 CY - Berlin, Gemany DA - 11.11.2022 KW - Transition metal KW - Phosphates KW - Non-classical crystallization KW - In-situ SAXS/WAXS KW - Cryo-TEM PY - 2022 AN - OPUS4-56479 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Chambers, Aaron T1 - Synthesis of functionalized ZIF nanoparticles for effective composite formation N2 - A presentation looking at ZIF-8 nanoparticles and functionalising them for more effective ZIF composite formation. T2 - UoB/BAM mini conference CY - Birmingham, UK DA - 06.10.2022 KW - MOF composite KW - 2PP KW - ZIF-8 KW - Nanoparticles PY - 2022 AN - OPUS4-56482 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bonse, Jörn A1 - Ayerdi, Jon J. A1 - Slachciak, Nadine A1 - Gradt, Thomas A1 - Krüger, Jörg A1 - Zabala, A. A1 - Spaltmann, Dirk T1 - Ultrakurzpulslaser induzierte Oxidschichten zur Reduktion von Reibung und Verschleiß auf Metalloberflächen N2 - Die Reduktion von Reibung und Verschleiß in technischen Systemen bietet ein großes Potenzial zur Reduktion von CO2-Emissionen. Dieser Beitrag diskutiert die Erzeugung und tribologische Charakterisierung von Ultrakurzpuls-generierten Nano- und Mikrostrukturen auf Metallen (Stahl, Titan). Besonderes Augenmerk wird dabei auf die Rolle der laserinduzierten Oxidschicht im Zusammenspiel mit verschleißreduzierenden Additiven in ölbasierten Schmiermitteln gerichtet. T2 - Workshop "Nachhaltigkeit durch Tribologische Schichten" - Europäische Forschungsgesellschaft Dünne Schichten e.V. CY - Karlsruhe, Germany DA - 17.05.2022 KW - Laser-induzierte periodische Oberflächenstrukturen KW - Reibungsreduktion KW - Verschleißreduktion KW - Oberflächenmodifikation KW - Oxidation KW - Additive PY - 2022 AN - OPUS4-54849 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mehri, S. A1 - Kolmangadi, Mohamed Aejaz A1 - Dyre, J.C. A1 - Ingebrigtsen, T.S. T1 - Lines of invariant physics in the isotropic phase of the discotic Gay-Berne model N2 - The Gay-Berne model is studied numerically with a choice of parameters allowing for the formation of a discotic liquid crystal at low temperatures. We show that the model has strong virial potential-energy correlations in the isotropic phase at high temperatures, i.e., it obeys the criterion for the existence of isomorphs, which are curves of approximately invariant structure and dynamics. These properties are demonstrated to be approximately invariant in reduced units along the isomorph studied. The isomorph is described well by the constant density-scaling exponent 11.5, a number that is significantly larger than the density-scaling exponents of various Lennard-Jones models that are always below 6. KW - Liquid Crystal KW - Molecular Dynamics PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-547611 DO - https://doi.org/10.1016/j.nocx.2022.100085 VL - 14 SP - 1 EP - 7 PB - Elsevier B.V. AN - OPUS4-54761 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bugel, S. A1 - Hahnel, M. A1 - Kunde, T. A1 - de Sousa Amadeu, Nadar A1 - Sun, Y. A1 - Spieß, A. A1 - Beglau, T. H. Y. A1 - Janiak, C. A1 - Schmidt, B. M. T1 - Synthesis and Characterization of a Crystalline Imine-Based Covalent Organic Framework with Triazine Node and Biphenyl Linker and Its Fluorinated Derivate for CO2/CH4 Separation N2 - A catalyst-free Schiff base reaction was applied to synthesize two imine-linked covalent organic frameworks (COFs). The condensation reaction of 1,3,5-tris-(4-aminophenyl)triazine (TAPT) with 4,4′-biphenyldicarboxaldehyde led to the structure of HHU-COF-1 (HHU = Heinrich-Heine University). The fluorinated analog HHU-COF-2 was obtained with 2,2′,3,3′,5,5′,6,6′-octafluoro-4,4′-biphenyldicarboxaldehyde. Solid-state NMR, infrared spectroscopy, X-ray photoelectron spectroscopy, and elemental analysis confirmed the successful formation of the two network structures. The crystalline materials are characterized by high Brunauer–Emmett–Teller surface areas of 2352 m2/g for HHU-COF-1 and 1356 m2/g for HHU-COF-2. The products of a larger-scale synthesis were applied to prepare mixed-matrix membranes (MMMs) with the polymer Matrimid. CO2/CH4 permeation tests revealed a moderate increase in CO2 permeability at constant selectivity for HHU-COF-1 as a dispersed phase, whereas application of the fluorinated COF led to a CO2/CH4 selectivity increase from 42 for the pure Matrimid membrane to 51 for 8 wt% of HHU-COF-2 and a permeability increase from 6.8 to 13.0 Barrer for the 24 wt% MMM. KW - MOF KW - Filter PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-547632 DO - https://doi.org/10.3390/ma15082807 SN - 1996-1944 VL - 15 IS - 8 SP - 1 EP - 18 PB - MDPI AN - OPUS4-54763 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hülagü, Deniz A1 - Tobias, Charlie A1 - Gojani, Ardian B. A1 - Rurack, Knut A1 - Hodoroaba, Vasile-Dan A1 - Hülagü, Deniz T1 - Towards automated scanning electron microscopy image analysis of core-shell microparticles for quasi-3D determination of the surface roughness N2 - Core-shell (CS) particles have been increasingly used for a wide range of applications due to their unique properties by merging individual characteristics of the core and the shell materials. The functionality of the designed particles is strongly influenced by their surface roughness. Quantitative evaluation of the roughness of CS microparticles is, however, a challenging task for Scanning Electron Microscopy (SEM). The SEM images contain two-dimensional (2D) information providing contour roughness data only from the projection of the particle in the horizontal plane. This study presents a practical procedure to achieve more information by tilting the sample holder, hence allowing images of different areas of a single particle to be recorded at different orientations under the same view angle. From the analysis of these images, quasi three-dimensional (3D) information is obtained. Three types of home-made particles were investigated: i) bare polystyrene (PS) particles, ii) PS particles decorated with a first magnetic iron oxide (Fe3O4) nanoparticle shell forming CS microbeads, iii) PS/Fe3O4 particles closed with a second silica (SiO2) shell forming core-shell-shell (CSS) microbeads. A series images of a single particle were taken with stepwise tilted sample holder up to 10° by an SEM with high-resolution and surface sensitive SE-InLens® mode. A reliable analysis tool has been developed by a script in Python to analyze SEM images automatically and to evaluate profile roughness quantitatively, for individual core-shell microparticles. Image analysis consists of segmentation of the images, identifying contour and the centre of the particle, and extracting the root mean squared roughness value (RMS-RQ) of the contour profile from the particle projection within a few seconds. The variation in roughness from batch-to-batch was determined with the purpose to set the method as a routine quality check procedure. Flow cytometry measurements provided complementary data. Measurement uncertainties associated to various particle orientations were also estimated. T2 - ICASS 5th International Conference on Applied Surface Science CY - Palma, Mallorca, Spain DA - 25.04.2022 KW - Core-shell particles KW - Image analysis KW - Roughness KW - Scanning electron microscopy PY - 2022 AN - OPUS4-54774 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mishmastnehi, Moslem A1 - Stawski, Tomasz T1 - Crystals of Gypsum in Hands of Masters N2 - The microstructure of most Seljuk and Ilkhanid stucco decorations consists of micrometer-sized crystals of gypsum. The stucco-masters of these periods (neither nowadays stucco-masters) were not able to directly control the properties of these tiny crystals with their hands or centimeter-sized tools. There are, however, traces of chaîne opératoire accumulated in the materialistic body of these pieces, some of which could be explored through an interdisciplinary approach. Such an investigation requires very careful in situ observation of the macrostructure, and scientific analyses of the material to discover part of the production process for each body of stucco. Furthermore, there are deterioration factors, some of which are not yet fully understood, and should be identified using modern analytical instruments. These damaging factors could easily affect the micro and macro structure of a stucco decoration, influencing our interpretation. The concept of chaîne opératoire reframes our questions about the production process and probable dating technique of Seljuk and Ilkhanid stuccoes, while analyses of labmade replicas and historic materials enhance our understanding and interpretation of these materials. Here we present the results of such a study for a large body of Seljuk and Ilkhanid stucco decorations at various sites in Iran, and present the potential of this approach as a new perspective in this field of research. T2 - Stucco in the Architecture of Iran and Neighbouring Lands CY - Bamberg, Germany DA - 04.05.2022 KW - Gypsum KW - Stuccos KW - Crystallization PY - 2022 AN - OPUS4-54782 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zänker, Steffen A1 - Scholz, G. A1 - Marquardt, Julien A1 - Emmerling, Franziska T1 - Structural changes in Ba-compounds of different hardness induced by high-energy ball milling – evidenced by 137Ba NMR and X-ray powder diffraction N2 - Changes in the global bulk and local structures, of three different barium compounds (BaZrO3, BaF2, and BaFCl),were induced by mechanical milling and followed using X-ray powder diffraction (PXRD), subsequent microstructure analysis, and 137Ba solid state NMR spectroscopy. Harder materials like BaZrO3 experience significantly higher structural changes upon milling than softer materials like BaF2. Moreover, soft materials with layered structures, like BaFCl, show a pronounced structural change during the milling process. By combining PXRD and solid state NMR, detailed information on the changes to the global and local structures were obtained, which are of interest for mechanochemical synthesis, mechanically treated catalysts or ionic conductors. KW - Mechanochemistry KW - X-ray diffraction KW - Solid state NMR PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-547397 DO - https://doi.org/10.1002/zaac.202200026 SN - 0044-2313 VL - 648 IS - 10 SP - 1 EP - 8 PB - Wiley-VCH CY - Weinheim AN - OPUS4-54739 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Flatken, M. A. A1 - Radicchi, E. A1 - Wendt, R. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Härk, E. A1 - Pascual, J. A1 - Mathies, F. A1 - Shargaieva, O. A1 - Prause, A. A1 - Dallmann, A. A1 - De Angelis, F. A1 - Hoell, A. A1 - Abate, A. T1 - Role of the Alkali Metal Cation in the Early Stages of Crystallization of Halide Perovskites N2 - ABX3 metal halide perovskites revolutionized the research and development of new optoelectronics, including solar cells and light-emitting diodes. Processing polycrystalline thin films from precursor solutions is one of the core advantages of these materials since it enables versatile and cost-effective manufacturing. The perovskite film morphology, that is, continuous substrate coverage and low surface roughness, is of paramount importance for highly efficient solar cells and optoelectronic devices in general. Controlling the chemistry of precursor solutions is one of the most effective strategies to manage the perovskite film morphology. Herein, we show the fundamental influence of the A-site cation composition on the perovskite precursor arrangement and the consequent film formation. Extended X-ray absorption fine structure spectroscopy and small-angle X-ray scattering give unprecedented insights into the complex structural chemistry of the perovskite precursors and, in particular, their repulsive interactions as a crucial parameter for colloidal stability. Combining these techniques with in situ grazing incidence wide-angle X-ray scattering during thin-film formation allows us to identify the mechanism for using alkali metals as a decisive criterion to control the colloidal stability of the perovskite precursor and thus the thin-film morphology. We illustrate the fundamental principle behind the systematic use of alkali metals regardless of whether they are incorporated in the lattice or not. Hence, this work provides tools to selectively control the morphology and crystal growth in present and future systems KW - MAPbI3 perovskites KW - Halide Perovskites KW - X-ray absorption spectroscopy PY - 2022 DO - https://doi.org/10.1021/acs.chemmater.1c03563 SN - 0897-4756 VL - 34 IS - 3 SP - 1121 EP - 1131 PB - American Chemical Society AN - OPUS4-54713 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bernges, T. A1 - Hanus, R. A1 - Wankmiller, B. A1 - Imasato, K. A1 - Lin, S. A1 - Ghidiu, M. A1 - Gerlitz, M. A1 - Peterlechner, M. A1 - Graham, S. A1 - Hautier, G. A1 - Pei, Y. A1 - Hansen, M. R. A1 - Wilde, G. A1 - Snyder, G. J. A1 - George, Janine A1 - Agne, M T. A1 - Zeier, W. G. T1 - Considering the Role of Ion Transport in Diffuson-Dominated Thermal Conductivity N2 - Next-generation thermal management requires the development of low lattice thermal conductivity materials, as observed in ionic conductors. For example, thermoelectric efficiency is increased when thermal conductivity is decreased. Detrimentally, high ionic conductivity leads to thermoelectric device degradation. Battery safety and design also require an understanding of thermal transport in ionic conductors. Ion mobility, structural complexity, and anharmonicity have been used to explain the thermal transport properties of ionic conductors. However, thermal and ionic transport are rarely discussed in direct comparison. Herein, the ionic conductivity of Ag+ argyrodites is found to change by orders of magnitude without altering the thermal conductivity. Thermal conductivity measurements and two-channel lattice dynamics modeling reveal that the majority of Ag+ vibrations have a non-propagating diffuson-like character, similar to amorphous materials. It is found that high ionic mobility is not a requirement for diffuson-mediated transport. Instead, the same bonding and structural traits that can lead to fast ionic conduction also lead to diffuson-mediated transport. Bridging the fields of solid-state ionics and thermal transport, it is proposed that a vibrational perspective can lead to new design strategies for functional ionic conducting materials. As a first step, the authors relate the so-called Meyer-Neldel behavior in ionic conductors to phonon occupations. KW - Diffusons KW - DFT KW - Phonons KW - Thermoelectrics PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-547140 DO - https://doi.org/10.1002/aenm.202200717 SN - 1614-6832 VL - 12 IS - 22 SP - 1 EP - 13 PB - Wiley VHC-Verlag AN - OPUS4-54714 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bonse, Jörn A1 - Mezera, Marek A1 - Florian, Camilo A1 - Krüger, Jörg A1 - Gräf, S. T1 - Laser-Induced Periodic Surface Structures: when Maxwell meets Marangoni N2 - Laser-Induced Periodic Surface Structures (LIPSS, ripples) are a universal phenomenon and can be generated in a contactless, single-step process on almost any material upon irradiation of solids with intense laser radiation. Nowadays, processing rates of up to m^2/min are enabling new industrial applications in medicine, optics, tribology, biology, etc. Depending on the specific type of LIPSS, their structural sizes typically range from several micrometers down to less than 100 nanometers – far beyond the optical diffraction limit – while their orientations exhibit a clear correlation with the local polarization direction of the laser radiation. From a theoretical point of view, however, a controversial and vivid debate has emerged during the last two decades, whether LIPSS originate from electromagnetic effects (seeded already during the laser irradiation) – or whether they emerge from matter reorganization processes, i.e. distinctly after the laser irradiation. This presentation reviews the currently existent theories of LIPSS. A focus is laid on the historic development of the fundamental ideas, their corresponding mathematical descriptions and numerical implementations, along with a comparison and critical assessment of the different approaches. T2 - 16th International Conference on Laser Ablation (COLA 2021/22) CY - Matsue, Japan DA - 24.04.2022 KW - Laser-induced periodic surface structures (LIPSS) KW - Laser ablation KW - Theoretical modelling KW - Electromagnetic scattering KW - Hydrodynamics PY - 2022 AN - OPUS4-54716 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Michalchuk, Adam A1 - Morrison, C. T1 - From lattice vibrations to molecular dissociation N2 - The ease with which an energetic material can be initiated by mechanical impact is a critical parameter directing material safety and application. While impact sensitivity metrics are traditionally derived experimentally, recent developments have highlighted that the phenomenon is amenable to first principles simulation. In this chapter, we will outline a fully ab initio approach to predict the relative impact sensitivities of energetic materials based on the mechanochemical principles that link the impact event to vibrational energy transfer. This mechanism is key to rationalizing how a mechanical impact—which deposits energy into the low-frequency lattice vibrations—results in a molecular response. By simulating the vibrational energy levels (the so-called phonon density of states, PDOS) using first-principles computational methods (typically dispersion-corrected plane-wave density functional theory, PW-DFT) we can calculate the relative rate of energy propagation from the delocalized low-energy lattice vibrations through to the localized molecular modes. The latter traps the energy, which eventually results in bond rupture through heightened vibrational excitation. This method, based on vibrational up-pumping, offers a route toward predicting the impact sensitivities of a broad range of energetic materials, provided the crystal structure of the compound (or salt or co-crystal) is known. While it does not offer insight into the sensitizing roles undoubtedly played by crystal defects or grain boundaries, it does provide a level of understanding at the molecular and crystal packing levels. Correspondingly, this approach offers a feedback mechanism to chemists and materials scientists to guide the design of new materials with desired impact sensitivity behavior. KW - Energetic materials KW - Density functional theory KW - Material design PY - 2022 DO - https://doi.org/10.1016/B978-0-12-822971-2.00010-3 VL - 22 SP - 215 EP - 232 PB - Elsevier B.V. AN - OPUS4-54717 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Yildirim, Arda A1 - Krause, Christina A1 - Huber, P. A1 - Schönhals, Andreas T1 - Multiple glassy dynamics of a homologous series of triphenylene-based columnar liquid crystals – A study by broadband dielectric spectroscopy and advanced calorimetry N2 - Hexakis(n-alkyloxy)triphenylene) (HATn) consisting of an aromatic triphenylene core and alkyl side chains are model discotic liquid crystal (DLC) systems forming a columnar mesophase. In the mesophase, the molecules of HATn self-assemble in columns, which has one-dimensional high charge carrier mobility along the columns. Here, a homologous series of HATn with different length of the alkyl chain (n = 5,6,8,10,12) is investigated using differential scanning calorimetry (DSC), broadband dielectric spectroscopy (BDS) and advanced calorimetric techniques including fast scanning calorimetry (FSC) and specific heat spectroscopy (SHS). The investigation of the phase behavior was done utilizing DSC experiments and the influence of the alkyl chain length on the phase behavior was revealed. By the dielectric investigations probing the molecular mobility, a c-relaxation due to localized fluctuations as well as two glassy dynamics, the acore- and aalkyl-relaxation, were observed in the temperature range of the plastic crystalline phase. Moreover, the observed glassy dynamics were further studied employing advanced calorimetry. All observed relaxation processes are attributed to the possible specific molecular fluctuations and discussed in detail. From the results a transition at around n = 8 from a rigid constrained (n = 5,6) to a softer system (n = 10,12) was revealed with increasing alkyl chain length. A counterbalance of two competing effects of a polyethylene-like behavior of the alkyl chains in the intercolumnar domains and self-organized confinement is discussed in the context of a hindered glass transition. KW - Discotic liquid crystals KW - Broadband dielectric spectroscopy KW - Advanced calorimetry PY - 2022 DO - https://doi.org/10.1016/j.molliq.2022.119212 VL - 358 SP - 1 EP - 10 PB - Elsevier B.V. AN - OPUS4-54721 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kolmangadi, Mohamed Aejaz A1 - Schönhals, Andreas T1 - Side Chain length dependent dynamics and conductivity of Ionic Liquid crystals N2 - We investigate the molecular dynamics and electrical conductivity for a homologous series of linear shaped guanidinium based cyclic ILCs that vary in alkyl chain length, CLCRs (R = 8, 10, 12, 14, 16) by employing broadband dielectric spectroscopy (BDS), and calorimetry comprised of Fast Scanning Calorimetry (FSC) and temperature modulated FSC (TMFSC). Besides conductivity at high temperatures, the dielectric dispersion reveals two relaxation modes: the fast γ and the slow α1 relaxation. The former is assigned to the localized fluctuations while the latter is due to segmental dynamics of the alkyl chains. The γ mode slows down for long chain length CLCs (12,14,16) compared to their shorter analogues. Calorimetric investigation reveals one process, the α2 process, for all ILCs. The α2 process for CLC10, 12, and 14 has a similar temperature dependence as the dielectric α1 relaxation, while for the CLC8 and 10, it's shifted to a higher temperature. For all CLCRs, the absolute values of DC conductivity increase by 4 orders of magnitude at the transition from the plastic crystalline to hexagonal columnar phase. This increase is due to the change in the underlying conduction mechanism from delocalized electron hopping in the crystalline phase to one-dimensional ion mobility in the columnar phase. The glassy dynamics shifts to higher temperatures with increasing alkyl chain length. Conversely, the DC conductivity drops by 3 orders of magnitude from CLC8 to CLC16. T2 - APS March Meeting 2022 CY - Chicago, IL, USA DA - 13.03.2022 KW - Glass transition KW - Conductivity KW - Fast Scanning Calorimetry KW - Dynamics PY - 2022 AN - OPUS4-54760 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Aree, T. A1 - McMonagle, C. J. A1 - Michalchuk, Adam A1 - Chernyshov, D. T1 - Low-frequency lattice vibrations from atomic displacement parameters of a-FOX-7, a high energy density material N2 - Highly anharmonic thermal vibrations may serve as a source of structural instabilities resulting in phase transitions, chemical reactions and even the mechanical disintegration of a material. Ab initio calculations model thermal motion within a harmonic or sometimes quasi-harmonic approximation and must be complimented by experimental data on temperature-dependent vibrational frequencies. Here multi-temperature atomic displacement parameters (ADPs), derived from a single-crystal synchrotron diffraction experiment, are used to characterize low-frequency lattice vibrations in the alpha-FOX-7 layered structure. It is shown that despite the limited quality of the data, the extracted frequencies are reasonably close to those derived from inelastic scattering, Raman measurements and density functional theory (DFT) calculations. Vibrational anharmonicity is parameterized by the Grüneisen parameters, which are found to be very different for in-layer and out-of-layer vibrations. KW - Energetic Materials KW - DFT KW - Structural dynamics KW - X-ray diffraction PY - 2022 DO - https://doi.org/10.1107/S2052520622002700 SN - 2052-5206 VL - 78 SP - 376 EP - 384 PB - Wiley-Blackwell CY - Oxford AN - OPUS4-54832 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krüger, Jörg A1 - Legall, Herbert A1 - Bonse, Jörn T1 - X-ray hazards and radiation protection aspects in ultrashort laser processing N2 - Ultrashort pulse laser micromachining at repetition rates of several hundreds of kHz allows a cost-effective high precision manufacturing, which makes this method attractive for many industrial applications. Upon exceeding a critical laser intensity, hard X-ray radiation is generated as a side effect. Even if the emitted X-ray dose per laser pulse is low, for currently available high-repetition-rate laser systems the accumulated X-ray dose becomes significant and radiation safety must be considered. Influences of the processing parameters are discussed and radiation protection aspects will be outlined T2 - AKL’22 – International Laser Technology Congress CY - Aachen, Germany DA - 04.05.2022 KW - Ultrashort pulse laser processing KW - X-ray emission KW - Radiation protection PY - 2022 AN - OPUS4-54805 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - EMPIR nPSize - Improved Traceability Chain of Nanoparticle Size Measurement - What nPSize can offer to ISO/TC 229? N2 - The main outcomes of the EMPIR project nPSize are presented and the suitability of the new capabilities, e.g. reference materials, sample preparation protocols, measurement procedures, and data analysis, to be standardized and implemented in accredited analytical laboratories is discussed. Complementation and/or filling gaps of published and ongoing standardisation projects on size, shape and number concentration measurements under ISO/TC 229/JWG 2 are offered. The two VAMAS inter-laboratory comparisons resulted from the nSPize project and just started under TWA 34 Nanoparticle Populations (Projects #15 and #16) of bipyramidal TiO2 anatase and bimodal SiO2 nanoparticles are presented in detail. T2 - Interim Meeting of ISO/TC 229 Nanotechnologies - Strategy and Metrology Group CY - Online meeting DA - 09.05.2022 KW - Nanoparticles KW - Particle size distribution KW - Inter-laboratory comparison KW - Electron microscopy KW - AFM KW - SAXS KW - ISO/TC229 PY - 2022 AN - OPUS4-54819 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Advanced Characterization of the Surface Morphology and Chemistry within nano@BAM N2 - Both essential aspects of the surface of solid matter, its morphology and chemistry, are studied traditionally at BAM starting in the 60’s with different cyclical research focus areas, mostly related either to applicative research or method development. In the recent years, the focus has shifted almost exclusively to the nano-analytics of advanced materials such as complex nanoparticles, (ultra)thin films/coatings, nanocomposites, 2D materials, energy materials, etc. This is also the reason why BAM has established recently the new Competence Center nano@BAM (www.bam.de/Navigation/DE/Themen/Material/Nanotechnologie/sichere-nanomaterialien.html) with the five sub-fields nanoCharacterisation, nanoMaterial, nanoSafety, nanoData and nanoTechnology. The link to the BAM central guidelines to the safety in technology and chemistry is given by the development of reference products such as reference measurement procedures, reference (nano)materials, and newly reference data sets. Thus, an internationally well-networked group in surface analysis has been established @BAM, with regular contributions to integral analytical characterization with metrological and standardization background. Examples of newly developed methodical approaches will be given with an emphasis on correlative nano-analysis of morphology and chemistry of nanomaterials. Correlative imaging by STEM-in-SEM with high-resolution SEM and EDX, and further with AFM or the new technique TKD (Transmission Kikuchi Diffraction) will be explained on various examples of nanostructures, both as starting materials and embedded/functionalized nanoparticles in products. The unique analytical benefits of the Auger electron probe as a veritable nano-tool for surface chemistry will be highlighted. The panoply of advanced surface characterization methods @BAM is completed by discussing examples of hybrid analysis of the bulk of nanomaterials by X-ray Spectroscopy with the highest surface-sensitive methods X-ray Photoelectron Spectroscopy (XPS) and Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS). Particularly for the analysis of the surface chemistry of nanostructures, such as the completeness of the shells of core-shell nanoparticles or in-depth and lateral gradients of chemistry within mesoporous thin layers, the latter methods are inherent. Other special developments like approaches for the quantitative determination of the roughness of particle surface by electron microscopy or for the quantitative determination of the porosity of thin mesoporous layers by electron probe microanalysis (EPMA) with SEM will be presented. T2 - Seminar of the Academic Centre for Materials and Nanotechnology CY - Online meeting DA - 12.05.2022 KW - Nanoparticles KW - Thin films KW - Nano Characterisation KW - Nanomaterials KW - Surface morphology KW - Surface chemistry PY - 2022 UR - https://www.agh.edu.pl/en/info/article/seminar-advanced-characterization-of-the-surface-morphology-and-chemistry-within-nanobam/ AN - OPUS4-54820 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Chambers, M. S. A1 - Hunter, R. D. A1 - Hollamby, M. J. A1 - Pauw, Brian Richard A1 - Smith, A. J. A1 - Snow, T. A1 - Danks, A. E. A1 - Schnepp, Z. T1 - In Situ and Ex Situ X‑ray Diffraction and Small-Angle X‑ray Scattering Investigations of the Sol−Gel Synthesis of Fe3N and Fe3C N2 - Iron nitride (Fe3N) and iron carbide (Fe3C) nanoparticles can be prepared via sol−gel synthesis. While sol−gel methods are simple, it can be difficult to control the crystalline composition, i.e., to achieve a Rietveld-pure product. In a previous in situ synchrotron study of the sol−gel synthesis of Fe3N/Fe3C, we showed that the reaction proceeds as follows: Fe3O4 → FeOx → Fe3N → Fe3C. There was considerable overlap between the different phases, but we were unable to ascertain whether this was due to the experimental setup (side-on heating of a quartz capillary which could lead to thermal gradients) or whether individual particle reactions proceed at different rates. In this paper, we use in situ wide- and small-angle X-ray scattering (wide-angle X-ray scattering (WAXS) and small-angle X-ray scattering (SAXS)) to demonstrate that the overlapping phases are indeed due to variable reaction rates. While the initial oxide nanoparticles have a small range of diameters, the size range expands considerably and very rapidly during the oxide−nitride transition. This has implications for the isolation of Rietveld-pure Fe3N, and in an extensive laboratory study, we were indeed unable to isolate phasepure Fe3N. However, we made the surprising discovery that Rietveld-pure Fe3C nanoparticles can be produced at 500 °C with a sufficient furnace dwell time. This is considerably lower than the previous reports of the sol−gel synthesis of Fe3C nanoparticles. KW - Small-angle X-ray Scattering KW - SAXS KW - Diffraction KW - XRD KW - Scattering KW - Sol-gel KW - Iron nitride KW - Nanoparticles KW - Iron carbide KW - Catalyst KW - In-situ KW - Ex-situ KW - Synthesis KW - Synchrotron PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-548226 DO - https://doi.org/10.1021/acs.inorgchem.1c03442 VL - 61 IS - 18 SP - 6742 EP - 6749 PB - ACS Publications CY - Washington AN - OPUS4-54822 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard A1 - Smales, Glen Jacob T1 - A quick intro to our NeXus format… N2 - A brief introduction is given into our data collection and organization procedure, and why we have settled on the HDF5-based NeXus format for describing experimental data. The links between NeXus and the SciCat data catalog is also provided, showing how the NeXus metadata is automatically added as searchable metadata in the catalog. T2 - NFDI NeXus Workshop CY - Online meeting DA - 17.03.2022 KW - Data management KW - Measurement organization KW - Measurement data KW - NFDI KW - FAIR KW - Open access KW - Data mining KW - Data tagging KW - Automated data tagging PY - 2022 AN - OPUS4-54823 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mazzeo, P. P. A1 - Prencipe, M. A1 - Feiler, Torvid A1 - Emmerling, Franziska A1 - Bacchi, A. T1 - On the mechanism of cocrystal mechanochemical reaction via low melting eutectic: A time-resolved in situ monitoring investigation N2 - Mechanochemistry has become a sustainable and attractive cost-effective synthetic technique, largely used within the frame of crystal engineering. Cocrystals, namely, crystalline compounds made of different chemical entities within the same crystal structure, are typically synthesized in bulk via mechanochemistry; however, whereas the macroscopic aspects of grinding are becoming clear, the fundamental principles that underlie mechanochemical cocrystallization at the microscopic level remain poorly understood. Time-resolved in situ (TRIS) monitoring approaches have opened the door to exceptional detail regarding mechanochemical reactions. We here report a clear example of cocrystallization between two solid coformers that proceeds through the formation of a metastable low melting binary eutectic phase. The overall cocrystallization process has been monitored by time-resolved in situ (TRIS) synchrotron X-ray powder diffraction with a customized ball milling setup, currently available at μ Spot beamline at BESSY-II, Helmholtz-Zentrum Berlin. The binary system and the low melting eutectic phase were further characterized via DSC, HSM, and VT-XRPD. KW - Mechanochemistry KW - In situ KW - Cocrystal PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-552977 DO - https://doi.org/10.1021/acs.cgd.2c00262 SN - 1528-7505 VL - 22 IS - 7 SP - 4260 EP - 4267 PB - ACS Publ. CY - Washington, DC AN - OPUS4-55297 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Macková, A. A1 - Jagerová, A. A1 - Lailik, O. A1 - Miksová, R. A1 - Poustka, D. A1 - Mistrík, J. A1 - Holý, V. A1 - Schütter, Jan David A1 - Kentsch, U. A1 - Marvan, P. A1 - Azarov, A. A1 - Galeckas, A. T1 - Combined Au/Ag nanoparticle creation in ZnO nanopillars by ion implantation for optical response modulation and photocatalysis N2 - ZnO nanopillars were implanted with Au-400 keV and Ag-252 keV ions with ion fluences from 1 × 10^15 cm^2 to 1 × 10^16 cm^2. We compared ZnO nanopillars solely implanted with Au-ions and dually-implanted with Au and Ag-ions. Rutherford Back-Scattering spectrometry (RBS) confirmed Ag and Au embedded in ZnO nanopillar layers in a reasonable agreement with theoretical calculations. A decreasing thickness of the ZnO nanopillar layer was evidenced with the increasing ion implantation fluences. Spectroscopic Ellipsometry (SE) showed a decrease of refractive index in the nanopillar parts with embedded Au, Ag-ions. XRD discovered vertical domain size decreasing with the proceeding radiation damage accumulated in ZnO nanopillars which effect was preferably ascribed to Au-ions. SE and diffuse reflectance spectroscopy (DRS) showed optical activity of the created nanoparticles at wavelength range 500 – 600 nm and 430 – 700 nm for the Au-implanted and Au, Ag-implanted ZnO nanopillars, respectively. Photoluminescence (PL) features linked to ZnO deep level emission appear substantially enhanced due to plasmonic interaction with metal nanoparticles created by Ag, Au-implantation. Photocatalytic activity seems to be more influenced by the nanoparticles presented in the layer rather than the surface morphology. Dual implantation with Ag, Au-ions enhanced optical activity to a larger extent without significant morphology deterioration as compared to the solely Au-ion implanted nanopillars. KW - ZnO nanopillars KW - Au/Ag nanoparticles, KW - Ion implantation KW - SPR KW - Doped ZnO nanostructures PY - 2022 DO - https://doi.org/10.1016/j.apsusc.2022.155556 SN - 0169-4332 VL - 610 SP - 1 EP - 13 PB - Elsevier B.V. AN - OPUS4-56306 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kricheldorf, H. A1 - Weidner, Steffen A1 - Meyer, A. T1 - Ring-expansion polymerization (REP) of L-lactide with cyclic tin catalysts – About formation of extended ring crystals and optimization of Tm and ΔHm N2 - L-Lactide was polymerized in bulk at 140 °C with three different cyclic tin catalysts and the time was varied from 1 d up to 14 d. The MALDI TOF spectra confirmed the formation of cyclic polylactides (PLAs) and displayed a characteristic change of peak intensity distribution with formation of a “saw tooth pattern”. This pattern confirms a previous hypothesis that cyclic PLAs tend to form crystallites with extended ring conformation and relatively smooth surface. This type of crystallites is formed under thermodynamic control by transesterification on the surface of the crystallites. In this way PLAs with extraordinarily high melting temperatures (Tm's up to 200.6 °C) and extraordinarily high melting enthalpy were obtained (ΔHm's up to 105 J g−1). These ΔHm values require a revision of the maximum ΔHm value calculated in the literature for ideal PLA crystals. KW - Polylactide KW - MALDI-TOF MS KW - ring-expansion polymerization PY - 2022 DO - https://doi.org/10.1016/j.polymer.2022.125516 SN - 0032-3861 VL - 263 SP - 125516 PB - Elsevier Ltd. AN - OPUS4-56338 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Pauw, Brian Richard T1 - dataMerge V0.1 - A statistics-aware binning and merging backend N2 - A tool for merging and/or rebinning single or multiple datasets to achieve a lower point density with best possible statistics. highly scriptable, CLI, no GUI Version 0.1: works but could do with a cleanup. Weighting by uncertainty currently always on, but should be optional for use as an azimuthal or radial averager KW - X-ray science KW - Image averaging KW - Dataset merging KW - Photon counting detectors KW - SAXS KW - SANS KW - X-ray scattering KW - X-ray diffraction PY - 2022 DO - https://doi.org/10.6084/m9.figshare.21591360 PB - Digital Science CY - Cambridge, MA, USA AN - OPUS4-56340 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin A1 - Kulow, A. A1 - Reinholz, Uwe A1 - de Oliveira Guilherme Buzanich, Ana A1 - Emmerling, Franziska A1 - Streli, C. A1 - Fittschen, U. E. A. A1 - Hampel, S. T1 - Energy Resolved Imaging with Coded Apertures N2 - Our aim is to develop a simple and inexpensive method for full field X-ray fluorescence imaging.We combine an energydispersive array detector with a coded aperture to obtain high resolut ion images. To obtain the information from the recorded image a reconstruction step is necessary. The reconstruction methods we have developed, were tested on simulated data and then applied to experimental data. The first tests were carried out at the BAMline @BESSY II. This method enables the simultaneous detection of multiple elements,which is important e.g. in the field of catalysis. T2 - SRI 2021 CY - Online meeting DA - 28.3.2022 KW - Synchrotron KW - BAMline KW - Machine Learning KW - Coded Aperture PY - 2022 AN - OPUS4-56298 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kulow, Anicó A1 - de Oliveira Guilherme Buzanich, Ana A1 - Reinholz, Uwe A1 - Emmerling, Franziska A1 - Hampel, S. A1 - Fittschen, UEA A1 - Streli, C. A1 - Radtke, Martin T1 - Reconstruction for coded aperture full-field x-ray fluorescence imaging N2 - X-ray fluorescence imaging is a well-established tool in materials characterization. In this work, we present the adaption of coded aperture imaging to full-field X-ray fluorescence imaging at the synchrotron. Coded aperture imaging has its origins in astrophysics, and has several advantages: Coded apertures are relatively easy to fabricate, achromatic, allow a high photon throughput, and high angular acceptance. Coded aperture imaging is a two-step-process, consisting of the measurement process and a reconstruction step. Different programs have been written, for the raytracing/forward projection and the reconstruction. Experiments with coded aperture in combination with a Color X-ray Camera and an energy-dispersive area detector, have been conducted at the BAMline. Measured samples were successfully reconstructed, and gave a 9.1-fold increase in count rate compared to a polycapillary optic. KW - Synchrotron KW - BAMline KW - Coded Aperture PY - 2022 SN - 1097-0002 VL - 65 SP - 57 EP - 70 PB - Cambridge University Press CY - Cambridge AN - OPUS4-56350 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bonse, Jörn A1 - Krüger, Jörg T1 - Structuring of thin films by ultrashort laser pulses N2 - Modern life and global communication would not be possible without technologically tailored thin films; they are omnipresent in daily life applications. In most cases, the films are deposited entirely at the carrying substrates in a specific processing step of the device or sample. In some cases, however, removal or modification must be performed locally, i.e., site-controlled and material selective through an additional laser processing step. For that ultrashort laser pulses with durations in the femtosecond and picosecond range can provide unique advantages and capabilities in industrially scalable schemes. This article reviews the current state of the research and corresponding industrial transfer related to the structuring of thin films by ultrashort pulsed lasers. It focuses on the pertinent historic developments, reveals the relevant physical and chemical effects, explores the ultimate limits, and discusses selected industrial and scientific applications. KW - Thin films KW - Laser processing KW - Ultrashort lasers KW - Laser damage KW - Femtosecond laser ablation PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-565732 DO - https://doi.org/10.1007/s00339-022-06229-x SN - 0947-8396 SN - 1432-0630 VL - 129 IS - 1 SP - 1 EP - 38 PB - Springer CY - Berlin AN - OPUS4-56573 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -