TY - JOUR A1 - Al-Terkawi, Abdal-Azim A1 - Prinz, Carsten A1 - Scholz, Gudrun A1 - Kemnitz, Erhard A1 - Emmerling, Franziska T1 - Ca-, Sr-, and Ba-Coordination polymers based on anthranilic acid via mechanochemistry N2 - Ca-, Sr-, and Ba-Based coordination polymers (CPs) were prepared mechanochemically by milling metal-hydroxide samples with anthranilic acid (oABAH). {[Ca(oABA)2(H2O)3]}n consists of one-dimensional polymeric chains that are further connected by a hydrogen-bonding network. {[Sr(oABA)2(H2O)2]·H2O}n is a one-dimensional CP in which water molecules bridge Sr2+ ions and increase the dimensionality by building an extended network. {[Ba(oABA)2(H2O)]}n crystallizes as a two-dimensional CP comprising one bridging water molecule. The cation radii influence the inorganic connectivity and dimensionality of the resulting crystal structures. The crystal structures were refined from powder X-ray diffraction data using the Rietveld method. The local coordination environments were studied via extended X-ray absorption fine structure (EXAFS) measurements. The compounds were further characterized using comprehensive analytical methods such as elemental analysis, thermal analysis, MAS NMR, imaging, and dynamic vapor sorption (DVS) measurements. Compounds 1, 2, and 3 exhibit small surface areas which decrease further after thermal annealing experiments. All compounds exhibit a phase transformation upon heating, which is only reversible in 3. KW - Mechanochemistry KW - XRD PY - 2019 DO - https://doi.org/10.1039/c9dt00991d SN - 1477-9226 SN - 1477-9234 VL - 48 IS - 19 SP - 6513 EP - 6521 PB - Royal Society of Chemistry AN - OPUS4-48014 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Akhmetova, Irina A1 - Schuzjajew, K. A1 - Wilke, M. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Rademann, K. A1 - Roth, C. A1 - Emmerling, Franziska T1 - Synthesis, characterization and in situ monitoring of the mechanochemical reaction process of two manganese(II)-phosphonates with N-containing ligands N2 - Two divalent manganese aminophosphonates, manganese mono (nitrilotrimethylphosphonate) (MnNP3) and manganese bis N-(carboxymethyl)iminodi(methylphosphonate)) (Mn(NP2AH)2), have been prepared by mechanochemical synthesis and characterized by powder X-ray diffraction (PXRD). The structure of the novel compound Mn(NP2AH)2 was determined from PXRD data. MnNP3 as well as Mn(NP2AH)2 exhibits a chain-like structure. In both cases, the manganese atom is coordinated by six oxygen atoms in a distorted octahedron. The local coordination around Mn was further characterized by extended X-ray absorption fine structure. The synthesis process was followed in situ by synchrotron X-ray diffraction revealing a three-step reaction mechanism. The asprepared manganese(II) phosphonates were calcined on air. All samples were successfully tested for their suitability as catalyst material in the oxygen evolution reaction. KW - Mechanochemistry KW - In situ KW - XRD PY - 2018 DO - https://doi.org/10.1007/s10853-018-2608-6 SN - 0022-2461 SN - 1573-4803 VL - 53 IS - 19 SP - 13390 EP - 13399 PB - Springer Science + Business Media B.V. AN - OPUS4-45673 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Akhmetova, Irina A1 - Schutjajew, Konstantin A1 - Roth, Christina A1 - Emmerling, Franziska T1 - Mechanochemical synthesis of metal phosphonates N2 - The exploration of metal phosphonates chemistry has gained great interest during the last decades, because of their structural diversity. Transition metal phosphonates are promising candidates for an application as electrocatalysts in oxygen evolution reactions (OER). Here, we present the in situ investigation of mechanochemical syntheses of different manganese phosphonates by synchrotron X-ray diffraction. Nitrilotri(methylenephosphonic acid) and N,N-Bis(phosphonomethyl)glycine were chosen as ligands. The liquid-assisted milling process can be divided into three steps, including an amorphous stage. One of the products has not been obtained by classical solution chemistry before. These metal phosphonates and/or their derivatives are considered to be active in electrochemical energy conversion. The verification of their applicability is one of the topics of our resent research. T2 - Fundamental Bases of Mechanochemical Technologies CY - Novosibirsk, Russia DA - 25.06.2018 KW - Metal phosphonates KW - Mechanochemistry KW - PXRD KW - Thermography PY - 2018 AN - OPUS4-46996 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Akhmetova, Irina A1 - Emmerling, Franziska A1 - Schutjajew, Konstantin A1 - Roth, Christina T1 - In situ investigation of milling reactions and structure determination of the products using X-ray diffraction N2 - Mechanochemistry is a versatile approach for green and fast synthesis of pure substances. By milling the reactants, various organic, inorganic, and metal-organic compounds can be obtained in high yields. Although mechanochemistry is widely used, the underlying mechanisms are not fully understood making mechanochemical reactions difficult to predict. Metal phosphonates are metal-organic compounds accessible by grinding. Because of their structural diversity, the exploration of the chemistry of metal phosphonates has gained considerable interest during the last decades. Transition metal phosphonates are promising candidates for an application as electrocatalysts in oxygen evolution reaction (OER). Here, we present the in situ investigation of the mechanochemical synthesis of a manganese(II)-phosphonate by synchrotron X-ray diffraction and thermography. The product has not been obtained by classical solution chemistry before and its crystal structure was determined from PXRD data. The milling process can be divided into different steps, with the product crystallization corresponding with the highest temperature rise. The activity of this metal phosphonate towards OER was measured and is presented here. T2 - International School of Crystallography - 52nd Course: Quantum Crystallography CY - Erice, Italy DA - 1.06.2018 KW - Metal phosphonates KW - Mechanochemistry KW - PXRD KW - OER KW - Thermography PY - 2018 AN - OPUS4-46998 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Akhmetova, Irina A1 - Haferkamp, Sebastian A1 - Schutjajew, Konstantin A1 - Roth, Christina A1 - Emmerling, Franziska T1 - In situ investigation of mechanochemical syntheses of manganese phosphonates with N-containing ligands N2 - Mechanochemistry is a versatile approach for green and fast synthesis of pure substances. The exploration of the chemistry of metal phosphonates has gained considerable interest during the last decades due to their structural diversity. We synthesized manganese phosphonates in milling reactions. The mechanochemical reactions were investigated in situ to reveal the underlying mechanisms. T2 - Joint BER II and BESSY II User Meeting CY - Berlin, Germany DA - 05.12.2018 KW - Metal phosphonates KW - Mechanochemistry KW - PXRD KW - In situ KW - Thermography PY - 2018 AN - OPUS4-46999 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ahmed, R. A1 - Vaishampayan, A. A1 - Cuellar-Camacho, J. L. A1 - Wight, D. J. A1 - Donskyi, Ievgen A1 - Unger, Wolfgang A1 - Grohmann, E. A1 - Haag, R. A1 - Wagner, O. T1 - Multivalent Bacteria Binding by Flexible Polycationic Microsheets Matching Their Surface Charge Density N2 - Aiming at the overall negative surface charge of bacteria, a new strategy of antibacterial agents based on large polymer-modified graphene oxide (GO) sheets is assessed. The presented flexible, polycationic Sheets match the size and charge density of the Escherichia coli surface charge density (2 × 1014 cm−2). These matching parameters create an unspecific but very strong bacteria adsorber by multivalent, electrostatic attraction. Their interaction with bacteria is visualized via atomic force and confocal microscopy and shows that they effectively bind and wrap around E. coli cells, and thereby immobilize them. The incubation of Gram-negative and -positive bacteria (E. coli and methicillin-resistant Staphylococcus aureus, MRSA) with these polycationic sheets leads to the inhibition of proliferation and a reduction of the colony forming bacteria over time. This new type of antibacterial agent acts in a different mode of Action than classical biocides and could potentially be employed in medicinal, technical, or agriculture applications. The presented microsheets and their unspecific binding of cell interfaces could further be employed as adsorber material for bacterial filtration or immobilization for imaging, analysis, or sensor technologies. KW - Surface charge KW - Bacteria KW - Graphene oxide KW - Escherichia coli KW - XPS PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-509651 DO - https://doi.org/10.1002/admi.201902066 VL - 7 IS - 15 SP - 1902066 PB - WILEY-VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-50965 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Acosta-Zepeda, C. A1 - Saavedra, S. A1 - Bonse, Jörn A1 - Haro-Poniatowski, E. T1 - Modelling of single UV nanosecond pulsed laser surface modifications of silicon N2 - Irradiation with a single spatially Gaussian-shaped nanosecond laser pulse in the melting regime can result in a characteristic annular change in the surface morphology of crystalline silicon. This has been verified experimentally in a variety of situations, where dimple-shaped surface topographies are produced. In a recent work we have investigated the induced changes in the surface topography upon exposure to wavelengths in the visible and near infrared spectral region. Irradiation in the UV requires a more detailed analysis due to the enhanced absorption of the material. In the present analysis, we determine under which conditions our previous model can be used and the corresponding results are presented. KW - Laser KW - Silicon KW - Surface modification PY - 2020 DO - https://doi.org/10.1088/1555-6611/ab9b2c SN - 1555-6611 SN - 1054-660X VL - 30 IS - 8 SP - 086003-1 EP - 086003-4 PB - IOP Publishing / Astro Ltd CY - Bristol, United Kingdom AN - OPUS4-51022 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Acosta-Zepeda, C. A1 - Saavedra, P. A1 - Bonse, Jörn A1 - Haro-Poniatowski, E. T1 - Modeling of silicon surface topographies induced by single nanosecond laser pulse induced melt-flows N2 - Irradiation with a single nanosecond laser pulse in the melting regime can result in a characteristic change in the surface morphology of crystalline silicon. This has been verified experimentally in a variety of situations, where dimple-shaped surface topographies are produced. In this work, the dimple height, depth, and width are modeled following and extending in a more rigorous manner the approach of Wood and Giles [Phys. Rev. B 23, 2923–2942 (1981)] and that of Schwarz-Selinger and coworkers [Phys. Rev. B 64, 155323 (2001)], upon varying the laser irradiation parameters such as peak energy density, pulse duration, and wavelength. This is achieved with numerical simulations of one-dimensional heat flow as input to the analytical fluid-flow equations. KW - Nanosecond laser KW - Melting KW - Silicon KW - Fluid-flow PY - 2019 DO - https://doi.org/10.1063/1.5053918 SN - 0021-8979 SN - 1089-7550 VL - 125 IS - 17 SP - 175101-1 EP - 175101-9 PB - AIP Publishing CY - Melville, USA AN - OPUS4-47927 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Abusafia, A. A1 - Scheid, C. A1 - Meurer, Maren A1 - Altmann, Korinna A1 - Dittmer, U. A1 - Steinmetz, H. T1 - Microplastic sampling strategies in urban drainage systems for quantification of urban emissions based on transport pathways N2 - Tracking waterborne microplastic (MP) in urban areas is a challenging task because of the various sources and transport pathways involved. Since MP occurs in low concentrations in most wastewater and stormwater streams, large sample volumes need to be captured, prepared, and carefully analyzed. The recent research in urban areas focused mainly on MP emissions at wastewater treatment plants (WWTPs), as obvious entry points into receiving waters. However, important transport pathways under wet-weather conditions are yet not been investigated thoroughly. In addition, the lack of comprehensive and comparable sampling strategies complicated the attempts for a deeper understanding of occurrence and sources. The goal of this paper is to (i) introduce and describe sampling strategies for MP at different locations in a municipal catchment area under dry and wet-weather conditions, (ii) quantify MP emissions from the entire catchment and two other smaller ones within the bigger catchment, and (iii) compare the emissions under dry and wet-weather conditions. WWTP has a high removal rate of MP (>96%), with an estimated emission rate of 189 kg/a or 0.94 g/[population equivalents (PEQ · a)], and polyethylene (PE) as the most abundant MP. The specific dry-weather emissions at a subcatchment were ≈30 g/(PEQ · a) higher than in the influent of WWTP with 23 g/(PEQ · a). Specific wet-weather emissions from large sub-catchment with higher traffic and population densities were 1952 g/(ha · a) higher than the emissions from smaller catchment (796 g/[ha · a]) with less population and traffic. The results suggest that wet-weather transport pathways are likely responsible for 2–4 times more MP emissions into receiving waters compared to dry-weather ones due to tire abrasion entered from streets through gullies. However, more investigations of wet-weather MP need to be carried out considering additional catchment attributes and storm event characteristics. KW - Combined sewer system KW - Large volume samplers KW - Microplastic pollution KW - Separate sewer system KW - Stormwater retention tank PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-568271 DO - https://doi.org/10.1002/appl.202200056 SP - 1 EP - 12 PB - Wiley-VCH CY - Weinheim AN - OPUS4-56827 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abram, Sarah-Luise A1 - Mrkwitschka, Paul A1 - Prinz, Carsten A1 - Rühle, Bastian A1 - Haase, Oskar A1 - Kuchenbecker, Petra A1 - Löhmann, Oliver A1 - Hodoroaba, Vasile-Dan A1 - Bresch, Harald A1 - Resch-Genger, Ute T1 - Iron oxide nanoparticles as a reference material candidate for particle size measurements N2 - This poster presentation covers the development of iron oxide nanoparticles as reference material candidate in the context of the project "Nanoplattform". T2 - EMRS Spring Meeting CY - Online meeting DA - 31.05.2021 KW - Iron oxide nanoparticles KW - Reference material KW - Particle size KW - Transmission electron microscopy KW - Small angle x-ray scattering PY - 2021 AN - OPUS4-52773 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -