TY - JOUR A1 - Schulz, K. A1 - Schmack, R. A1 - Klemm, H. W. A1 - Kabelitz, Anke A1 - Schmidt, T. A1 - Emmerling, Franziska A1 - Kraehnert, R. T1 - Mechanism and kinetics of hematite crystallization in air: Linking bulk and surface models via mesoporous films with defined nanostructure N2 - Iron can form numerous oxides, hydroxides, and oxide−hydroxides. Despite their relevance, many of the transformation processes between these phases are still poorly understood. In particular the crystallization of quasi-amorphous hydroxides and oxide−hydroxides is difficult to assess, since typical diffraction and scattering methods provide only sampleaveraged information about the crystallized phases. We report a new approach for the investigation of the crystallization of oxide−hydroxides. The approach relies on model-type films that comprise a defined homogeneous nanostructure. The nanostructure allows quantitative linking of Information obtained by bulk-averaging diffraction techniques (XRD, SAXS) with locally resolved information, i.e., Domain sizes (SEM, TEM, LEEM) and phase composition (SAED). Using time-resolved imaging and diffraction we deduce mechanism and kinetics for the crystallization of ferrihydrite into hematite. Hematite forms via nucleation of hematite domains and subsequent Domain growth that terminates only upon complete transformation. A Johnson−Mehl−Avrami−Kolmogorov model describes the kinetics over a wide temperature range. The derived understanding enables the first synthesis of ferrihydrite films with ordered mesoporosity and quantitative control over the films’ hematite and ferrihydrite content. KW - Iron oxide KW - Crystallization KW - Mesoporous films KW - Nanostructure PY - 2017 DO - https://doi.org/10.1021/acs.chemmater.6b05185 SN - 0897-4756 SN - 1520-5002 VL - 29 IS - 4 SP - 1724 EP - 1734 AN - OPUS4-39690 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Wilrich, Cordula A1 - Schröder, Volkmar A1 - Brandes, E. A1 - Schmidt, Martin A1 - Wandrey, Peter-Andreas A1 - Mix, K.-H. A1 - Wehrstedt, Klaus-Dieter A1 - Bender, H. A1 - Stephan, U. A1 - Eberz, A. A1 - Steinbach, J. A1 - Stoessel, F. T1 - Plant and process safety - 2. Hazardous materials and process conditions N2 - "Ullmann's Encyclopedia of Industrial Chemistry" is the benchmark reference in chemistry and chemical and life science engineering, covering inorganic and organic chemicals, advanced materials, pharmaceuticals, polymers and plastics, metals and alloys, biotechnology and biotechnological products, food chemistry, process engineering and unit operations, analytical methods, environmental protection, and much more. The present article is part of the topic collection "Environmental Protection and Industrial Safety". It covers plant and process safety, focusing on hazardous materials and process conditions. KW - Flammable gases and vapors KW - Combustibility of liquids KW - Dust explosions KW - Explosive condensed substances KW - Harmful effects of substances KW - Exothermic and pressure-inducing chemical reactions PY - 2012 SN - 978-3-527-30673-2 DO - https://doi.org/10.1002/14356007.q20_q01 SP - 1 EP - 50 PB - Wiley-VCH CY - Weinheim AN - OPUS4-58108 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Everard, C.D. A1 - Schmidt, Martin A1 - McDonnell, K.P. A1 - Finnan, J. T1 - Heating processes during storage of Miscanthus chip piles and numerical simulations to predict self-ignition N2 - Miscanthus x Giganteus (Miscanthus) energy crop was examined at laboratory scale to assess its self-heating and self-ignition risks during storage. Chipped Miscanthus (18 mm) from February and March harvests, in 2012, were assessed as well as ground Miscanthus (3 mm) from the March harvest. February and March crops had moisture contents of 41.6 and 20.2%, respectively. Self-ignition temperatures were independent of moisture although moisture did affect the time from the beginning of storage until storage temperature was reached. Ground Miscanthus had lower self-ignition temperatures than chipped Miscanthus. Isothermal respirometric tests carried out showed increase risk of self-heating in the February crop compared to the March crop due to increased microbial activity. Numerical simulations were used to determine critical enhanced start temperatures, e.g. caused by microbial decomposition, of the stored Miscanthus. Safe storage conditions have been derived from the investigations. The numerical simulations demonstrated that self-ignition was possible in Miscanthus chip piles with a height greater than 6 m if there was significant heat release from microbiological activity. Reliable assessment of self-heating and self-ignition risks in large scale Miscanthus energy crop clamps or piles are required to prevent losses due to decomposition and fire damage. KW - Miscanthus x Giganteus KW - Hot storage test KW - Respirometric rates KW - Self-heating KW - Self-ignition KW - Numerical simulations KW - Biomass storage PY - 2014 DO - https://doi.org/10.1016/j.jlp.2014.06.003 SN - 0950-4230 SN - 1873-3352 VL - 30 SP - 188 EP - 196 PB - Butterworth CY - Guildford, Surrey AN - OPUS4-31149 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bier, A.K. A1 - Bognitzki, M. A1 - Schmidt, A. A1 - Greiner, A. A1 - Gallo, Emanuela A1 - Klack, Patrick A1 - Schartel, Bernhard T1 - Synthesis, properties, and processing of new siloxane-substituted poly(p-xylylene) via CVD N2 - The synthesis of a disiloxane-functionalized [2.2]paracyclophane and its polymerization to the corresponding siloxane-substituted poly(p-xylylene) via chemical vapor deposition (CVD) has been described. Because of the enhanced solubility of the siloxane substituted poly(p-xylylene) analysis of the molecular structure by NMR, molecular weight, and polydispersity by gel permeation chromatography (GPC), and processing by film casting as well as nanofiber formation by electrospinning was possible. Structural isomers were found by NMR which was expected due to the isomeric mixture of the precursor. High molecular weights at moderate polydispersities were found by GPC which was unexpected for a vapor phase deposition polymerization. The amorphous morphology in combination with a low glass transition temperature led to high elongation at break for the siloxane substituted poly(p-xylylene). Significant difference for the wetting versus water was found for as-deposited films, solution cast films, and nanofibers obtained by electrospinning with contact angles up to 135° close to superhydrophobic behavior. KW - Poly(p-xylylene) KW - Siloxane functionalized PPX KW - Chemical vapor deposition KW - Difunctionalized [2.2]paracyclophanes KW - Gorham process PY - 2012 DO - https://doi.org/10.1021/ma2021369 SN - 0024-9297 SN - 1520-5835 VL - 45 IS - 2 SP - 633 EP - 639 PB - American Chemical Society CY - Washington, DC AN - OPUS4-25466 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Everard, C.D. A1 - Finnan, J. A1 - McDonnell, K.P. A1 - Schmidt, Martin T1 - Evaluation of self-heating in Miscanthus x giganteus energy crop clamps and the implications for harvesting time N2 - Miscanthus x giganteus energy crop grown in Ireland was harvested on 21st of February and 28th of March 2012 to examine the effects of harvesting time on self-heating during storage of Miscanthus chips in clamps (98 m³) under weather sheltered conditions. There was a relatively large difference in moisture content, of 21.4%, between Miscanthus crop harvested in February and March (41.6 and 20.2%, respectively). Temperature evolution over a storage period of up to 125 days was monitored at different heights and distances from the centre within the clamps. Maximum temperature in the February constructed clamp reached 69 °C compared to 28 °C in the March constructed clamp. Microbial activity was monitored via carbon dioxide and oxygen gas measurements. The high moisture clamp showed higher microbial activity and a volume yield loss of 4.3% due to decomposition in the top section of the clamp. Quality indices post-storage were also assessed. Calorific values from Miscanthus sampled 1 m below the top surface were similar after storage for both February and March constructed clamps, i.e. 18.52 and 18.70 MJ kg-1, respectively. A reliable assessment of self-heating in Miscanthus chip clamps has important consequences for both self-ignition risk and biomass quality. KW - Self-heating KW - Miscanthus x giganteus KW - Biomass storage KW - Self-ignition KW - Biomass quality PY - 2013 DO - https://doi.org/10.1016/j.energy.2013.06.022 SN - 0360-5442 VL - 58 SP - 350 EP - 356 PB - Elsevier CY - Amsterdam [u.a.] AN - OPUS4-29054 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Franco de Carvalho, J. M. A1 - Defàveri, K- A1 - Castro Mendes, J. A1 - Schmidt, Wolfram A1 - Kühne, Hans-Carsten A1 - Fiorotti Peixoto, R. A. T1 - Influence of particle size-designed recycled mineral admixtures on the properties of cement-based composites N2 - In this work, engineered recycled mineral admixtures were obtained from four different industrial residues: basic oxygen furnace slag, iron ore tailings, quartz mining tailings and quartzite mining tailings. The grinding performance was evaluated in two different programs and the characterization included chemical and mineralogical composition, particle morphology, and physical properties. Performance evaluations were carried out in blended pastes and mortars, including flow properties, hydration kinetics, soundness, pozzolanic activity, and compressive strength. Coarser-than-cement admixtures allowed better flow performance, greater dimensional stability and more economical production, while finer-thancementn admixtures improved mechanical performance by both filler effect and cementing activity. KW - Engineered recycled mineral admixtures KW - Rheology KW - Hydration kinetics KW - Basic oxygen furnace slag KW - Iron ore tailings KW - Mining tailings PY - 2021 DO - https://doi.org/10.1016/j.conbuildmat.2020.121640 SN - 0950-0618 VL - 272 SP - 1 EP - 13 PB - Elsevier Ltd. AN - OPUS4-58255 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kim, K.J. A1 - Unger, Wolfgang A1 - Kim, J.W. A1 - Moon, D.W. A1 - Gross, Thomas A1 - Hodoroaba, Vasile-Dan A1 - Schmidt, Dieter A1 - Wirth, Thomas A1 - Jordaan, W. A1 - van Staden, M. A1 - Prins, S. A1 - Zhang, L. A1 - Fujimoto, T. A1 - Song, X.P. A1 - Wang, H. T1 - Inter-laboratory comparison: quantitative surface analysis of thin Fe-Ni alloy films N2 - An international interlaboratory comparison of the measurement capabilities of four National Metrology Institutes (NMIs) and one Designated Institute (DI) in the determination of the chemical composition of thin Fe-Ni alloy films was conducted via a key comparison (K-67) of the Surface Analysis Working Group of the Consultative Committee for Amount of Substance. This comparison was made using XPS (four laboratories) and AES (one laboratory) measurements. The uncertainty budget of the measured chemical composition of a thin alloy film was dominated by the uncertainty of the certified composition of a reference specimen which had been determined by inductively coupled plasma mass spectrometry using the isotope dilution method. Pilot study P-98 showed that the quantification using relative sensitivity factors (RSFs) of Fe and Ni derived from an alloy reference sample results in much more accurate result in comparison to an approach using RSFs derived from pure Fe and Ni films. The individual expanded uncertainties of the participants in the K-67 comparison were found to be between 2.88 and 3.40 atomic %. The uncertainty of the key comparison reference value (KCRV) calculated from individual standard deviations and a coverage factor (k) of 2 was 1.23 atomic %. KW - Quantification KW - Fe-Ni alloy KW - Uncertainty KW - Key comparison KW - Traceability PY - 2012 DO - https://doi.org/10.1002/sia.3795 SN - 0142-2421 SN - 1096-9918 VL - 44 IS - 2 SP - 192 EP - 199 PB - Wiley CY - Chichester AN - OPUS4-24505 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schmidt, B.V.K.J. A1 - Fechler, N. A1 - Falkenhagen, Jana A1 - Lutz, J.-F. T1 - Controlled folding of synthetic polymer chains through the formation of positionable covalent bridges N2 - Covalent bridges play a crucial role in the folding process of sequence-defined biopolymers. This feature, however, has not been recreated in synthetic polymers because, apart from some simple regular arrangements (such as block co-polymers), these macromolecules generally do not exhibit a controlled primary structure—that is, it is difficult to predetermine precisely the sequence of their monomers. Herein, we introduce a versatile strategy for preparing foldable linear polymer chains. Well-defined polymers were synthesized by the atom transfer radical polymerization of styrene. The controlled addition of discrete amounts of protected maleimide at precise times during the synthesis enabled the formation of polystyrene chains that contained positionable reactive alkyne functions. Intramolecular reactions between these functions subsequently led to the formation of different types of covalently folded polymer chains. For example, tadpole (P-shaped), pseudocyclic (Q-shaped), bicyclic (8-shaped) and knotted (α-shaped) macromolecular origamis were prepared in a relatively straightforward manner. KW - Copolymerization KW - Chain folding KW - SEC KW - NMR KW - FT-IR KW - LAC KW - MALDI PY - 2011 DO - https://doi.org/10.1038/NCHEM.964 SN - 1755-4330 SN - 1755-4349 VL - 3 SP - 234 EP - 238 PB - Nature Publishing Group CY - London, UK AN - OPUS4-23888 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -