TY - JOUR
A1 - Szymoniak, Paulina
A1 - Kolmangadi, Mohamed A.
A1 - Böhning, Martin
A1 - De Souza, N. R.
A1 - Juranyi, F.
A1 - Zorn, R.
A1 - Schönhals, Andreas
T1 - Inelastic and Quasielastic Neutron Scattering on Polynorbornenes with Bulky Carbocyclic Side groups
N2 - This study investigates the molecular mobility and vibrational properties of polynorbornenes with bulky carbocyclic side groups using inelastic and quasielastic neutron scattering techniques. The polymers, synthesized via metathesis and addition polymerization, exhibit varying degrees of microporosity, which ignificantly influences their gas separation performance. By inelastic neutron scattering experiments, it could be shown that all considered polymers have excess contributions to the low frequency vibrational density of states known as the Boson peak. The maximum frequency of the Boson peak correlates to the microporosity of the polymers.
This correlation supports the sound wave interpretation of the Boson peak, suggesting that the microporous structure enhances the compressibility of the material at a microscopic length scale. The molecular mobility, particularly the methyl group rotation, was characterized using elastic scans and quasielastic neutron scattering. The study revealed a temperature dependent relaxation process, with the onset of molecular fluctuations observed around 200 K for the polymer containing methyl groups. For the polymer having no methyl groups only elastic scattering is observed. The methyl group rotation was analyzed in terms of a jump diffusion in a threefold potential with three equivalent energy minima. This leads to an almost correct description of the q dependence of the elastic incoherent scattering function when the number of hydrogen nuclei undergoing the methyl group rotation is considered. It was further evidenced that the fraction of methyl undergoing the methyl group rotation increases with increasing temperature.
KW - Polymers of Intrinsic Microporosity
KW - Neutron scattering
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-630297
DO - https://doi.org/10.1016/j.polymer.2025.128358
SN - 1873-2291
VL - 328
SP - 241
PB - Elsevier Ltd.
AN - OPUS4-63029
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Roters, F.
A1 - Aslam, A.
A1 - Bai, Y.
A1 - Büschelberger, M.
A1 - Bulert, K.
A1 - Butz, A.
A1 - Hickel, Tilmann
A1 - Jogi, T.
A1 - Klitschke, S.
A1 - Martin, M.
A1 - Meyer, L.-P.
A1 - Morand, L.
A1 - Nahshon, Y.
A1 - Radtke, N.
A1 - Saikia, Ujjal
A1 - Trondl, A.
A1 - Wessel, A.
A1 - Zierep, P.
A1 - Helm, D.
T1 - StahlDigital: Ontology-Based Workflows for the Steel Industry
N2 - The innovative strength of the steel industry is based on the mastery of microstructure–property relationships. Digital workflows can largely contribute to this aim by making the complexity of workflows reproducible and their execution user independent. In this work, the tools and workflows developed in the project StahlDigital as part of the German MaterialDigital initiative are presented and application examples are provided. A steel ontology builds the
foundation for data collection and storage as well as for the semantic description of experimental and simulation data processing workflows. A dataspace powered by the Dataspace Management System (DSMS) digitally represents such workflows and manages data along them in a Findable, Accessible, Interoperable, Reusable manner aiming to derive new knowledge. Experimental data processed via DSMS can be further evaluated and used as input for simulation workflows. The simulations included in such workflows are run by the workflow system pyiron, which has been semantically extended in StahlDigital for this purpose.
KW - Steel
KW - Rolling
KW - Multiscale simulation
KW - Ontology
KW - Workflow
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-627187
DO - https://doi.org/10.1002/adem.202402148
SN - 1527-2648
SP - 1
EP - 13
PB - Wiley VHC-Verlag
AN - OPUS4-62718
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 - Grengg, C.
A1 - Koraimann, G.
A1 - Ukrainczyk, N.
A1 - Rudic, O.
A1 - Luschnig, S.
A1 - Gluth, Gregor
A1 - Radtke, Martin
A1 - Dietzel, M.
A1 - Mittermayr, F.
T1 - Cu- and Zn-doped alkali activated mortar – Properties and durability in (bio)chemically aggressive wastewater environments
N2 - Metakaolin-based alkali activated mortars (AAM) - with and without CuSO4·5H2O and ZnO addition (mass ratio Mn+/solid binder 0.08% to 1.7%) - were casted and exposed within an extensive long-term field campaign over the period of 20 months to a sewer basin, strongly affected by biogenic acid corrosion. (Un-)exposed AAM were tested regarding their physicochemical and microstructural properties, bioreceptivity and overall durability. Metal addition led to a retarding effect during alkali-activation reaction, as well as to an increase in open porosity of up to 3.0% and corresponding lower compressive strength of up to 10.9%. Reduced microbial colonization and diversity were observed on AAM with Cu, while Zn addition led to increased biodiversity. We propose that the observed higher durability of Cu-doped AAM is due to antibacterial effects and associated reduction of biogenic acid production, superseding overall negative effects of metal-dosage on physical material properties. Observed lower durability of Zn-doped AAM was related to combined negative physicochemical and microbial effects.
KW - Microbially induced corrosion
KW - Alkali-activated materials
KW - Biogenic acid corrosion
KW - Biogene Schwefelsäurekorrosion
KW - MIC
PY - 2021
DO - https://doi.org/10.1016/j.cemconres.2021.106541
SN - 0008-8846
VL - 149
SP - 1
EP - 15
PB - Elsevier
CY - Oxford
AN - OPUS4-53070
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 - JOUR
A1 - Förste, F.
A1 - Bauer, L.
A1 - Streeck, C.
A1 - Radtke, Martin
A1 - Reinholz, Uwe
A1 - Kadow, D.
A1 - Keil, C.
A1 - Mantouvalou, I.
T1 - Quantitative Analysis and 2D/3D Elemental Imaging of Cocoa Beans Using X‑ray Fluorescence Techniques
N2 - As an important raw material for the confectionery industry, the cocoa bean (Theobroma cacao L.) has to meet certain legal requirements in terms of food safety and maximum contaminant levels in order to enter the cocoa market. Understanding the enrichment and distribution of essential minerals but also toxic metals is of utmost importance for improving the nutritional quality of this economically important raw food material. We present three X-ray fluorescence (XRF) techniques for elemental bio-imaging of intact cocoa beans and one additional XRF technique for quantitative analysis of cocoa pellets. The interrelation of all the methods presented gives a detailed picture of the content and 3D-resolved distribution of elements in complete cocoa beans for the first time.
KW - BAMline
KW - Synchrotron
KW - XRF
KW - CXC
KW - Cocoa
PY - 2023
DO - https://doi.org/10.1021/acs.analchem.2c05370
VL - 95
SP - 5627
EP - 5635
PB - ACS Publications
AN - OPUS4-57832
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Grengg, C.
A1 - Gluth, Gregor
A1 - Mittermayr, F.
A1 - Ukrainczyk, N.
A1 - Bertmer, M.
A1 - de Oliveira Guilherme Buzanich, Ana
A1 - Radtke, Martin
A1 - Leis, A.
A1 - Dietzel, M.
T1 - Deterioration mechanism of alkali-activated materials in sulfuric acid and the influence of Cu: A micro-to-nano structural, elemental and stable isotopic multi-proxy study
N2 - In this study, a multi-proxy approach combining 29Si, 27Al and 1H MAS-NMR, FEG-EPMA, XANES at the Cu K-edge and XRD analytics with hydrochemical tools such as ICP-OES analyses, oxygen-isotope signatures, and thermodynamic modelling was applied to K-silicate-activated metakaolin specimens - with and without CuSO4·5H2O addition - exposed to sulfuric acid at pH = 2 for 35 days. The results revealed a multistage deterioration mechanism governed by (i) acid diffusion, (ii) leaching of K-A-S-H, (iii) microstructural damage related to precipitation of expansive (K,Ca,Al)-sulfate-hydrate phases (iv) complete dissolution of the K-A-S-H framework, (v) and formation of silica gel in the outermost corroded regions. Copper ions were mainly located in layered spertiniite-chrysocolla-like phases in the as-cured materials. The results demonstrate an overall negative effect of Cu addition on chemical material durability, implying that the reported higher durability of Cu-doped AAM in biocorrosion environments can be best explained by bacteriostatic effects.
KW - Alkali-activated materials
KW - Acid resistance
KW - Microbially induced corrosion
KW - MIC
PY - 2021
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-520567
DO - https://doi.org/10.1016/j.cemconres.2021.106373
SN - 0008-8846
VL - 142
SP - 1
EP - 15
PB - Elsevier
CY - Oxford
AN - OPUS4-52056
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Gomes, Bruna F.
A1 - Prokop, Martin
A1 - Bystron, Tomas
A1 - Loukrakpam, Rameshwori
A1 - Melke, Julia
A1 - Lobo, Carlos M. S.
A1 - Fink, Michael
A1 - Zhu, Mengshu
A1 - Voloshina, Elena
A1 - Kutter, Maximilian
A1 - Hoffmann, Hendrik
A1 - Yusenko, Kirill V.
A1 - de Oliveira Guilherme Buzanich, Ana
A1 - Röder, Bettina
A1 - Bouzek, Karel
A1 - Paulus, Beate
A1 - Roth, Christina
T1 - Following Adsorbed Intermediates on a Platinum Gas Diffusion Electrode in H3PO3-Containing Electrolytes Using In Situ X-ray Absorption Spectroscopy
N2 - One of the challenges of high-temperature polymer electrolyte membrane fuel cells is the poisoning of the Pt catalystwith H3PO4. H3PO4 is imbibed into the routinely used polybenzimidazole-based membranes, which facilitate Proton conductivity in the temperature range of 120−200 °C. However, when leached out of the membrane by water produced during operation, H3PO4 adsorbs on the Pt catalyst surface, blocking the active sites and hindering the oxygen reduction reaction (ORR).
The reduction of H3PO4 to H3PO3, which occurs at the anode due to a combination of a low potential and the presence of gaseous H2, has been investigated as an additional important contributing factor to the observed poisoning effect. H3PO3 has an affinity toward adsorption on Pt surfaces even greater than that of H2PO4 −. In this work, we investigated the poisoning effect of both H3PO3 and H3PO4 using a half-cell setup with a gas diffusion electrode under ambient conditions. By means of in situ X-ray absorption spectroscopy, it was possible to follow the signature of different species adsorbed on the Pt nanoparticle catalyst (H, O, H2PO4 −, and H3PO3) at different potentials under ORR conditions in various electrolytes (HClO4, H3PO4, and H3PO3). It was found that H3PO3 adsorbs in a pyramidal configuration P(OH)3 through a Pt−P bond. The competition between H3PO4 and H3PO3 adsorption was studied, which should allow for a better understanding of the catalyst poisoning mechanism and thus assist in the development of strategies to mitigate this phenomenon in the future by minimizing H3PO3 generation by, for example, improved catalyst design or adapted operation conditions or changes in the electrolyte composition.
KW - H3PO4 life cycle
KW - XAS
KW - In situ coupling
KW - High-temperature fuel cells
KW - H3PO3,
KW - Δμ XANES
PY - 2022
DO - https://doi.org/10.1021/acscatal.2c02630
SN - 2155-5435
VL - 12
IS - 18
SP - 11472
EP - 11484
PB - American Chemical Society (ACS)
AN - OPUS4-64733
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - C. Pardo Pérez, L.
A1 - Arndt, A.
A1 - Stojkovikj, S.
A1 - Y. Ahmet, I.
A1 - T. Arens,, J.
A1 - Dattila, F.
A1 - Wendt, R.
A1 - de Oliveira Guilherme Buzanich, Ana
A1 - Radtke, Martin
A1 - Davies, V.
A1 - Höflich, K.
A1 - Köhnen, E.
A1 - Tockhorn, P.
A1 - Golnak, R.
A1 - Xiao, J.
A1 - Schuck, G.
A1 - Wollgarten, M.
A1 - López, N.
A1 - T. Mayer, M.
T1 - Determining Structure-Activity Relationships in Oxide Derived CuSn Catalysts During CO2 Electroreduction Using X-Ray Spectroscopy
N2 - The development of earth-abundant catalysts for selective electrochemical CO2 conversion is a central challenge. Cu-Sn bimetallic catalysts can yield selective CO2 reduction toward either CO or formate. This study presents oxide-derived Cu-Sn catalysts tunable for either product and seeks to understand the synergetic effects between Cu and Sn causing these selectivity trends. The materials undergo significant transformations under CO2 reduction conditions, and their dynamic bulk and surface structures are revealed by correlating observations from multiple methods—X-ray absorption spectroscopy for in situ study, and quasi in situ X-ray photoelectron spectroscopy for surface sensitivity. For both types of catalysts, Cu transforms to metallic Cu0 under reaction conditions. However, the Sn speciation and content differ significantly between the catalyst types: the CO-selective catalysts exhibit a surface Sn content of 13 at. % predominantly present as oxidized Sn, while the formate-selective catalysts display an Sn content of ≈70 at. % consisting of both metallic Sn0 and Sn oxide species. Density functional theory simulations suggest that Snδ+ sites weaken CO adsorption, thereby enhancing CO selectivity, while Sn0 sites hinder H adsorption and promote formate production. This study reveals the complex dependence of catalyst structure, composition, and speciation with electrochemical bias in bimetallic Cu catalysts.
KW - Electrochemical CO2 conversion
KW - Cu catalysts
KW - X-ray absorption spectroscopy
PY - 2022
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-547116
DO - https://doi.org/10.1002/aenm.202103328
SN - 1614-6832
VL - 12
IS - 5
SP - 2103328
PB - Wiley-VCH GmbH
AN - OPUS4-54711
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - de Oliveira Guilherme Buzanich, Ana
A1 - Cakir, Cafer Tufan
A1 - Radtke, Martin
A1 - Haider, M. Bilal
A1 - Emmerling, Franziska
A1 - F. M. Oliveira, P.
A1 - Michalchuk, Adam
T1 - Dispersive x-ray absorption spectroscopy for time-resolved in situ monitoring of mechanochemical reactions
N2 - X-ray absorption spectroscopy (XAS) provides a unique, atom-specific tool to probe the electronic structure of solids. By surmounting long-held limitations of powder-based XAS using a dynamically averaged powder in a Resonant Acoustic Mixer (RAM), we demonstrate how time-resolved in situ (TRIS) XAS provides unprecedented detail of mechanochemical synthesis. The use of a custom-designed dispersive XAS (DXAS) setup allows us to increase the time resolution over existing fluorescence measurements from ∼15 min to 2 s for a complete absorption spectrum. Hence, we here establish TRIS-XAS as a viable method for studying mechanochemical reactions and sampling reaction kinetics. The generality of our approach is demonstrated through RAM-induced (i) bottom-up Au nanoparticle mechanosynthesis and (ii) the synthesis of a prototypical metal organic framework, ZIF-8. Moreover, we demonstrate that our approach also works with the addition of a stainless steel milling ball, opening the door to using TRIS-DXAS for following conventional ball milling reactions. We expect that our TRIS-DXAS approach will become an essential part of the mechanochemical tool box.
KW - In situ studies
KW - Dipsersive XAS
KW - Mechanochemistry
KW - Time-resolved
PY - 2022
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-567659
DO - https://doi.org/10.1063/5.0130673
SN - 1089-7690
VL - 157
IS - 21
SP - 1
EP - 12
PB - American Institute of Physics
CY - Melville, NY
AN - OPUS4-56765
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Guerra, M.F.
A1 - Neri, E.
A1 - Radtke, Martin
T1 - Gold leaf tesserae: tracing the origins of gold using synchrotron-based techniques
N2 - To gain insight into the possible origin of the gold used in the production of tesserae containing gold leaf less than 0.5 μm thick placed between two layers of glass, we propose a non-destructive synchrotron radiation (SR) XRF protocol based on sequential analysis under optimised analytical conditions. Using this protocol, trace element analysis is achieved with detection limits of 1–6 mg/kg. As Pt and Au have adjacent fluorescence energies, we tested the most challenging situation, when Pt is present in very low concentrations in gold. Data obtained by double-dispersive XRF (D2XRF) and μXRF for fourth–ninth-century mosaics decorating nine Eastern and Western religious buildings show that the Eastern and Western tesserae are made from different alloys.
However, these alloys are identical to those used to make gold leaf for gilding, because plastic deformation requires the use of gold alloys with high ductility and malleability. Although trace element composition of gold used in the concerned period is only available for coins, by comparing the amounts of Pt contained in the tesserae and in the coins we show that Roman tesserae are made from Roman gold, as described in the documentary sources. We observe for the Byzantine period the use of a Byzantine gold and of gold supposedly from different stages of recycling, and we suggest the use of Umayyad and Abbasid gold for the production of Islamic tesserae.
KW - Gold
KW - XRF
KW - Synchrotron
KW - BAMline
KW - D2XRF
KW - Tesserae
PY - 2023
DO - https://doi.org/10.1140/epjp/s13360-022-03638-y
SN - 2190-5444
VL - 138
IS - 2
SP - 1
EP - 15
AN - OPUS4-57208
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CHAP
A1 - Radtke, Martin
A1 - Reinholz, Uwe
A1 - Guerra, M.F.
A1 - Martinón-Torres, M.
A1 - Lemasson, Q.
A1 - Moignard, B.
A1 - Pacheco, C.
A1 - Pichon, L.
A1 - Macdonald, L.
A1 - Hess, M.
A1 - Tissot, I.
ED - Guerra, M. F.
ED - Martinón-Torres, M.
ED - Quirke, S.
T1 - Analytical approaches to Egyptian goldwork
N2 - The structure and composition of ancient gold objects retain information about their long history of manufacture, from the exploitation of the ore to the finishing touches, as well as evidence of their use, deposition, and degradation. By developing an efficient analytical strategy, it is possible to retrieve that information. This chapter sets the necessary foundation 131to explore fully the analytical results presented in the following chapters of this volume. The techniques employed in the analyses of the Egyptian jewellery are described and the analytical parameters provided. For more established techniques, only brief introductions are presented, while more recent developments are presented in greater detail.
KW - Gold
KW - Synchrotron
KW - D2XRF
KW - Egypt
PY - 2023
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-586039
DO - https://doi.org/10.17863/CAM.99681
SP - 131
EP - 191
AN - OPUS4-58603
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -