TY - JOUR A1 - Adam, Christian A1 - Peplinski, Burkhard A1 - Michaelis, Matthias A1 - Kley, Gerd A1 - Simon, Franz-Georg T1 - Thermochemical treatment of sewage sludge ashes for phosphorus recovery JF - Waste management N2 - Phosphorus (P) is an essential element for all living organisms and cannot be replaced. Municipal sewage sludge is a carrier of phosphorus, but also contains organic pollutants and heavy metals. A two-step thermal treatment is suggested, including mono-incineration of sewage sludge and subsequent thermochemical treatment of the ashes. Organic pollutants are completely destroyed by mono-incineration. The resulting sewage sludge ashes contain P, but also heavy metals. P in the ashes exhibits low bioavailability, a disadvantage in farming. Therefore, in a second thermochemical step, P is transferred into mineral phases available for plants, and heavy metals are removed as well. The thermochemical treatment was investigated in a laboratory-scale rotary furnace by treating seven different sewage sludge ashes under systematic variation of operational parameters. Heavy metal removal and the increase of the P-bioavailability were the focus of the investigation. The present experimental study shows that these objectives have been achieved with the proposed process. The P-bioavailability was significantly increased due to the formation of new mineral phases such as chlorapatite, farringtonite and stanfieldite during thermochemical treatment. KW - P-recovery KW - Sewage sludge ash KW - Thermochemical treatment KW - Mineral phases KW - X-ray diffraction PY - 2009 DO - https://doi.org/10.1016/j.wasman.2008.09.011 SN - 0956-053X VL - 29 IS - 3 SP - 1122 EP - 1128 PB - Pergamon Press CY - New York, NY AN - OPUS4-18605 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Allsop, N. A. A1 - Schönmann, A. A1 - Belaidi, A. A1 - Muffler, H.-J. A1 - Mertesacker, B. A1 - Bohne, W. A1 - Strub, Erik A1 - Röhrich, J. A1 - Lux-Steiner, M. C. A1 - Fischer, C.-H. T1 - Indium sulfide thin films deposited by the spray ion layer gas reaction technique JF - Thin solid films N2 - The Spray Ion Layer Gas Reaction (Spray-ILGAR) technique is a new variation on the ILGAR technique used to prepare chalcogenide thin films. High quality indium sulfide thin films were produced by Spray-ILGAR with an indirect bandgap of 2.2 eV and a high suitability for use as buffer layers in chalcopyrite solar cells. The process involves the cyclical spray deposition of an indium containing precursor layer followed by its conversion to sulfide using hydrogen sulfide gas. Analysis of the deposition reveals that the indium chloride based precursor is transported via the vapour phase from the spray droplets to the substrate surface. KW - Spray deposition KW - Indium sulfide KW - Ion layer gas reaction KW - ILGAR KW - X-ray diffraction KW - X-ray fluorescence KW - Deposition process PY - 2006 DO - https://doi.org/10.1016/j.tsf.2006.01.019 SN - 0040-6090 VL - 513 IS - 1-2 SP - 52 EP - 56 PB - Elsevier CY - Amsterdam AN - OPUS4-14267 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 JF - Acta crystallographica B 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 - JOUR A1 - Aßmus, Kristin A1 - Hübner, Wolfgang A1 - Pyzalla, A. A1 - Pinto, H.C. T1 - Die Entwicklung des Gefüges in der Verschleißspur bei Gleitverschleiß von FeCrNi-Legierungen JF - Tribologie und Schmierungstechnik KW - Rostfreier Stahl KW - Deformation KW - Transformation KW - Gefüge KW - Martensit KW - Röntgendiffraktion KW - Stainless steel KW - Microstructure KW - Martensite KW - X-ray diffraction PY - 2004 SN - 0724-3472 VL - 51 IS - 3 SP - 30 EP - 33 PB - Expert Verlag CY - Renningen AN - OPUS4-3789 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Becker, Amadeus A1 - Schröpfer, Dirk A1 - Kromm, Arne A1 - Kannengießer, Thomas T1 - Determination of residual stress evolution during repair welding of high-strength steel components JF - Forces in mechanics N2 - During the assembly of steel structures, unacceptable weld defects may be found. An economical solution is local thermal gouging of the affected areas and re-welding. Due to high shrinkage restraints of repair weld and sur- rounding structure, high global and local welding stresses superimpose, and may lead to cracking and component failure, especially in connection with the degraded microstructure and mechanical properties of high-strength steels during the repair process. Component-related investigations of high-strength steels (FOSTA P1311/ IGF20162N) focus on welding residual stress evolution during local thermal gouging and rewelding. In this study, repair welding of S500MLO (EN 10225) is carried out using in-situ digital image correlation (DIC) and ex- situ X-ray diffraction (XRD) to analyse strains and stresses. Self-restrained slit specimen geometries were identified representing defined rigidity conditions of repair welds of real components, which were quantified using the restraint intensity concept. The specimens were rewelded with constant welding heat control and parameters. Weld specimens exhibited significantly increased transverse residual stresses with higher transverse restraint intensities, in the weld metal, and in the heat affected zone. Transverse stresses along the weld seam decrease at the weld seam ends leading to different stress state during gouging and welding. XRD analysis of the longitudinal and transverse local residual stresses after cooling to RT showed a good comparability with global DIC analyses. KW - Repair-welding KW - High-strength steels KW - X-ray diffraction KW - Digital image correlation KW - Residual stresses PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-555672 DO - https://doi.org/10.1016/j.finmec.2022.100073 SN - 2666-3597 VL - 6 SP - 1 EP - 6 PB - Elsevier CY - Amsterdam AN - OPUS4-55567 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bjeoumikhov, A. A1 - Bjeoumikhova, Zemfira A1 - Riesemeier, Heinrich A1 - Radtke, Martin A1 - Wedell, R. T1 - Propagation of synchrotron radiation through nanocapillary structures JF - Physics letters A N2 - The propagation of synchrotron radiation through nanocapillary structures with channel sizes of 200 nm and periods in the micrometer size has been studied experimentally. It was shown that the propagation through individual capillary channels has a mode formation character. Furthermore it was shown that during the propagation through capillary channels the coherence of synchrotron radiation is partially conserved. Interference of beams propagating through different capillary channels is observed which leads to a periodically modulated distribution of the radiation intensity in a plane far from the exit of the structure. These investigations are of high relevance for the understanding of X-ray transmission through nanocapillaries and the appearance of wave properties at this size scale. KW - Polycapillary structure KW - Nanocapillary KW - X-ray optics KW - Wave properties KW - Synchrotron radiation KW - X-ray diffraction PY - 2007 DO - https://doi.org/10.1016/j.physleta.2007.01.092 SN - 0031-9163 SN - 0375-9601 VL - 366 IS - 4-5 SP - 283 EP - 288 PB - North-Holland Publ. Co. CY - Amsterdam AN - OPUS4-20580 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Burek, K. A1 - Dengler, J. A1 - Emmerling, Franziska A1 - Feldmann, Ines A1 - Kumke, M. U. A1 - Stroh, Julia T1 - Lanthanide Luminescence Revealing the Phase Composition in Hydrating Cementitious Systems JF - ChemistryOpen N2 - The hydration process of Portland cement in a cementitious system is crucial for development of the high-quality cementbased construction material. Complementary experiments of Xray diffraction analysis (XRD), scanning electron microscopy (SEM) and time-resolved laser fluorescence spectroscopy (TRLFS) using europium (Eu(III)) as an optical probe are used to analyse the hydration process of two cement systems in the absence and presence of different organic admixtures. We Show that different analysed admixtures and the used sulphate carriers in each cement system have a significant influence on the hydration process, namely on the time-dependence in the formation of different hydrate phases of cement. Moreover, the effect of a particular admixture is related to the type of sulphate carrier used. The quantitative information on the amounts of the crystalline cement paste components is accessible via XRD analysis. Distinctly different morphologies of ettringite and calcium-silicate-hydrates (C-S-H) determined by SEM allow visual conclusions about formation of these phases at particular ageing times. The TRLFS data provides information about the admixture influence on the course of the silicate reaction. The dip in the dependence of the luminescence decay times on the hydration time indicates the change in the structure of C-S-H in the early hydration period. Complementary information from XRD, SEM and TRLFS provides detailed information on distinct periods of the cement hydration process. KW - Cement admixtures KW - Cement hydration KW - Europium KW - Luminescence KW - SEM KW - X-ray diffraction PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-504842 DO - https://doi.org/10.1002/open.201900249 VL - 8 IS - 12 SP - 1441 EP - 1452 PB - Wiley-VCH AN - OPUS4-50484 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bär, S. A1 - Huber, G. A1 - Gonzalo, J. A1 - Perea, A. A1 - Munz, Martin T1 - Pulsed laser deposition of EU - Y2O3 thin films on (0001) alpha-Al2O3 JF - Applied physics A N2 - This paper focuses on the preparation and characterization of crystalline thin films of rare-earth-doped sesquioxides (Y2O3, Lu2O3) grown by pulsed laser deposition on single-crystal (0001) sapphire substrates. X-ray diffraction measurements show that the films with thicknesses between 1 nm and 500 nm were highly textured along the 111 direction. Using Rutherford backscattering analysis, the correct stoichiometric composition of the films was established. The emission and excitation spectra of europium-doped films with a thickness 100 nm look similar to those of the corresponding crystalline bulk material, whereas films with a thickness 20 nm show a completely different emission behavior. KW - Pulsed laser deposition KW - Integrated optical devices KW - X-ray diffraction KW - Atomic force microscopy KW - Luminescence PY - 2004 UR - http://www.sciencedirect.com/science/journal/0926860X DO - https://doi.org/10.1007/s00339-004-3029-8 SN - 0947-8396 VL - 80 IS - 2 SP - 209 EP - 216 PB - Springer CY - Berlin AN - OPUS4-5990 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - de Olivera, Paulo A1 - Michalchuk, Adam A1 - de Oliveira Guilherme Buzanich, Ana A1 - Bienert, Ralf A1 - Torresi, R. A1 - Camargo, P. A1 - Emmerling, Franziska T1 - Tandem X-ray absorption spectroscopy and scattering for in situ time-resolved monitoring of gold nanoparticle mechanosynthesis JF - ChemComm N2 - Current time-resolved in situ approaches limit the scope of mechanochemical investigations possible. Here we develop a new, general approach to simultaneously follow the evolution of bulk atomic and electronic structure during a mechanochemical synthesis. This is achieved by coupling two complementary synchrotron-based X-ray methods: X-ray absorption spectroscopy (XAS) and X-ray diffraction. We apply this method to investigate the bottom-up mechanosynthesis of technologically important Au micro and nanoparticles in the presence of three different reducing agents, hydroquinone, sodium citrate, and NaBH4. Moreover, we show how XAS offers new insight into the early stage generation of growth species (e.g. monomers and clusters), which lead to the subsequent formation of nanoparticles. These processes are beyond the detection capabilities of diffraction methods. This combined X-ray approach paves the way to new directions in mechanochemical research of advanced electronic materials. KW - Mechanochemistry KW - XANES KW - X-ray diffraction KW - Nano particles PY - 2020 DO - https://doi.org/10.1039/d0cc03862h SN - 1364-548X VL - 56 SP - 10329 EP - 10332 PB - Royal Society of Chemistry AN - OPUS4-51760 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dreßler, Martin A1 - Nofz, Marianne A1 - Malz, Frank A1 - Pauli, Jutta A1 - Jäger, Christian A1 - Reinsch, Stefan A1 - Scholz, G. T1 - Aluminum speciation and thermal evolution of aluminas resulting from modified Yoldas sols JF - Journal of solid state chemistry N2 - Aluminas resulting from sols prepared via a modified Yoldas procedure were studied with differential thermal analysis (DTA), differential thermal gravimetrie (DTG), 27Al nuclear magnetic resonance (27Al MAS NMR) and X-ray diffraction (XRD) concerning their thermal properties, aluminum speciation and phase content. Hydrolysis of aluminum-sec-butoxide in aluminum nitrate solutions allowed to prepare stable sols with varying NO3-/Al molar ratios, solids contents and pH values. Resulting sols contained different aluminum species including also Al13 polycations. Sol preparation conditions also determined aluminum speciation in solid products obtained after thermal treatments of gels obtained from these sols. Al13 polycations and AlO5 species were found to play an important role for thermally induced transformation from amorphous products via eta-Al2O3 to alpha-Al2O3. Intermediately formed eta-Al2O3 promotes the phase transformation to alpha-Al2O3. KW - Alumina KW - Modified Yoldas sols KW - 27Al nuclear magnetic resonance KW - Differential thermal analysis KW - X-ray diffraction PY - 2007 DO - https://doi.org/10.1016/j.jssc.2007.06.018 SN - 0022-4596 SN - 1095-726X VL - 180 IS - 9 SP - 2409 EP - 2419 PB - Elsevier CY - San Diego, Calif. AN - OPUS4-16189 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Duva, G. A1 - Pithan, L. A1 - Zeiser, C. A1 - Reisz, B. A1 - Dieterle, J. A1 - Hofferberth, B. A1 - Beyer, P. A1 - Bogula, L. A1 - Opitz, A. A1 - Kowarik, Stefan A1 - Hinderhofer, A. A1 - Gerlach, A. A1 - Schreiber, F. T1 - Thin-Film Texture and Optical Properties of Donor/Acceptor Complexes. Diindenoperylene/F6TCNNQ vs Alpha-Sexithiophene/ F6TCNNQ JF - The Journal of Physical Chemistry C N2 - In this work, two novel donor/acceptor (D/A) complexes, namely, diindenoperylene (DIP)/1,3,4,5,7,8-hexafluoro-tetracyanonaphthoquinodimethane (F6TCNNQ) and alpha-sexithiophene (6T)/F6TCNNQ, are studied. The D/A complexes segregate in form of π−π stacked D/A cocrystals and can be observed by X-ray scattering. The different conformational degrees of freedom of the donor molecules, respectively, seem to affect the thin-film crystalline texture and composition of the D/A mixtures significantly. In equimolar mixtures, for DIP/F6TCNNQ, the crystallites are mostly uniaxially oriented and homogeneous, whereas for 6T/F6TCNNQ, a mostly 3D (isotropic) orientation of the crystallites and coexistence of domains of pristine compounds and D/A complex, respectively, are observed. Using optical absorption spectroscopy, we observe for each of the two mixed systems a set of new, strong transitions located in the near-IR range below the gap of the pristine compounds: such transitions are related to charge-transfer (CT) interactions between donor and acceptor. The optical anisotropy of domains of the D/A complexes with associated new electronic states is studied by ellipsometry. We infer that the CT-related transition dipole moment is perpendicular to the respective π-conjugated planes in the D/A complex. KW - Optical properties KW - Molecular semiconductor KW - X-ray diffraction PY - 2018 DO - https://doi.org/10.1021/acs.jpcc.8b03744 SP - 18705 EP - 18714 PB - ACS AN - OPUS4-46400 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Epishin, A. A1 - Brückner, Udo A1 - Link, T. A1 - Fedelich, Bernard T1 - X-ray reflections from the Gamma/Gamma'-microstructure of nickel-base superalloys: effect of the plane tilting JF - International journal of materials research N2 - The shape of X-ray reflections from the cuboidal γ/γ'-microstructure was investigated. The measurements were performed on the 4th generation single-crystal nickel-base superalloy TMS138. It is shown that reflections from non-cubic crystallographic planes split not only in d-scale due to the different spacing of the γ- and γ'-lattices but also in the pole figure due to the tilting of γ-lattice planes. This tilting results from the elastic distortion of the γ-lattice caused by the γ/γ'-misfit. The results obtained are discussed under the methodical aspect of misfit measurement. KW - Nickel-base alloys KW - X-ray diffraction KW - Lattice distortion PY - 2010 DO - https://doi.org/10.3139/146.110315 SN - 1862-5282 VL - 101 IS - 5 SP - 589 EP - 593 PB - Carl Hanser CY - München AN - OPUS4-21512 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fankhänel, J. A1 - Silbernagl, Dorothee A1 - Ghasem Zadeh Khorasani, Media A1 - Daum, B. A1 - Kempe, A. A1 - Sturm, Heinz A1 - Rolfes, R. T1 - Mechanical properties of Boehmite evaluated by Atomic Force Microscopy experiments and Molecular Dynamic Finite Element simulations JF - Journal of Nanomaterials N2 - Boehmite nanoparticles show great potential in improving mechanical properties of fiber reinforced polymers. In order to predict the properties of nanocomposites, knowledge about the material parameters of the constituent phases, including the boehmite particles, is crucial. In this study, the mechanical behavior of boehmite is investigated using Atomic Force Microscopy (AFM) experiments and Molecular Dynamic Finite Element Method (MDFEM) simulations. Young’s modulus of the perfect crystalline boehmite nanoparticles is derived from numerical AFM simulations. Results of AFM experiments on boehmite nanoparticles deviate significantly. Possible causes are identified by experiments on complementary types of boehmite, that is, geological and hydrothermally synthesized samples, and further simulations of imperfect crystals and combined boehmite/epoxy models. Under certain circumstances, the mechanical behavior of boehmite was found to be dominated by inelastic effects that are discussed in detail in the present work.The studies are substantiated with accompanying X-ray diffraction and Raman experiments. KW - AFM KW - MDFEM KW - Nanocomposite KW - Epoxy KW - X-ray diffraction KW - Raman spectroscopy KW - Young’s modulus KW - Slippage of weakly linked layers PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-384230 UR - https://www.hindawi.com/journals/jnm/2016/5017213/#B26 DO - https://doi.org/10.1155/2016/5017213 VL - 2016 IS - Article ID 5017213 SP - 1 EP - 13 PB - Hindawi Publishing Corporation AN - OPUS4-38423 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Feiler, Torvid A1 - Bhattacharya, Biswajit A1 - Michalchuk, Adam A1 - Schröder, V. A1 - List-Kratochvil, E. A1 - Emmerling, Franziska T1 - Mechanochemical Syntheses of Isostructural Luminescent Cocrystals of 9-Anthracenecarboxylic Acid with two Dipyridines Coformers JF - Crystals N2 - Tuning and controlling the solid-state photophysical properties of organic luminophore are very important to develop next-generation organic luminescent materials. With the aim of discovering new functional luminescent materials, new cocrystals of 9-anthracene carboxylic acid (ACA) were prepared with two different dipyridine coformers: 1,2-bis(4-pyridyl)ethylene and 1,2-bis(4-pyridyl)ethane. The cocrystals were successfully obtained by both mechanochemical approaches and conventional solvent crystallization. The newly obtained crystalline solids were characterized thoroughly using a combination of single crystal X-ray diffraction, powder X-ray diffraction, Fourier-transform infrared spectroscopy, differential thermal analysis, and thermogravimetric analysis. Structural analysis revealed that the cocrystals are isostructural, exhibiting two-fold interpenetrated hydrogen bonded networks. While the O–H···N hydrogen bonds adopts a primary role in the stabilization of the cocrystal phases, the C–H···O hydrogen bonding interactions appear to play a significant role in guiding the three-dimensional assembly. Both π···π and C–H···π interactions assist in stabilizing the interpenetrated structure. The photoluminescence properties of both the starting materials and cocrystals were examined in their solid states. All the cocrystals display tunable photophysical properties as compared to pure ACA. Density functional theory simulations suggest that the modified optical properties result from charge transfers between the ACA and coformer molecules in each case. This study demonstrates the potential of crystal engineering to design solid-state luminescence switching materials through cocrystallization. KW - Cocrystal KW - Mechanochemical synthesis KW - Luminescence KW - X-ray diffraction KW - DFT calculation PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-518226 DO - https://doi.org/10.3390/cryst10100889 VL - 10 IS - 10 SP - 889 PB - MDPI AN - OPUS4-51822 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Feng, W. A1 - Gemming, T. A1 - Giebeler, L. A1 - Qu, J. A1 - Weinel, Kristina A1 - Agudo Jácome, Leonardo A1 - Büchner, B. A1 - Gonzalez-Martinez, I. T1 - Influence of magnetic field on electron beam-induced Coulomb explosion of gold microparticles in transmission electron microscopy JF - Ultramicroscopy N2 - In this work we instigated the fragmentation of Au microparticles supported on a thin amorphous carbon film by irradiating them with a gradually convergent electron beam inside the Transmission Electron Microscope. This phenomenon has been generically labeled as ‘‘electron beam-induced fragmentation’’ or EBIF and its physical origin remains contested. On the one hand, EBIF has been primarily characterized as a consequence of beam-induced heating. On the other, EBIF has been attributed to beam-induced charging eventually leading to Coulomb explosion. To test the feasibility of the charging framework for EBIF, we instigated the fragmentation of Au particles under two different experimental conditions. First, with the magnetic objective lens of the microscope operating at full capacity, i.e. background magnetic field 𝐵 = 2 T, and with the magnetic objective lens switched off (Lorenz mode), i.e. 𝐵 = 0 T. We observe that the presence or absence of the magnetic field noticeably affects the critical current density at which EBIF occurs. This strongly suggests that magnetic field effects play a crucial role in instigating EBIF on the microparticles. The dependence of the value of the critical current density on the absence or presence of an ambient magnetic field cannot be accounted for by the beam-induced heating model. Consequently, this work presents robust experimental evidence suggesting that Coulomb explosion driven by electrostatic charging is the root cause of EBIF. KW - Electron beam-induced fragmentation KW - Coulomb explosion KW - X-ray diffraction KW - Lorenz transmission electron microscopy KW - Electron beam-induced charging PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-600170 DO - https://doi.org/10.1016/j.ultramic.2024.113978 VL - 262 SP - 1 EP - 8 PB - Elsevier B.V. AN - OPUS4-60017 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Feng, Wen A1 - Gemming, Thomas A1 - Giebeler, Lars A1 - Qu, Jiang A1 - Weinel, Kristina A1 - Agudo Jácome, Leonardo A1 - Büchner, Bernd A1 - González-Martínez, Ignacio T1 - Influence of magnetic field on electron beam-induced Coulomb explosion of gold microparticles in transmission electron microscopy JF - Ultramicroscopy N2 - In this work we instigated the fragmentation of Au microparticles supported on a thin amorphous carbon film by irradiating them with a gradually convergent electron beam inside the Transmission Electron Microscope. This phenomenon has been generically labeled as “electron beam-induced fragmentation” or EBIF and its physical origin remains contested. On the one hand, EBIF has been primarily characterized as a consequence of beam-induced heating. On the other, EBIF has been attributed to beam-induced charging eventually leading to Coulomb explosion. To test the feasibility of the charging framework for EBIF, we instigated the fragmentation of Au particles under two different experimental conditions. First, with the magnetic objective lens of the microscope operating at full capacity, i.e. background magnetic field B = 2 T, and with the magnetic objective lens switched off (Lorenz mode), i.e. B = 0 T. We observe that the presence or absence of the magnetic field noticeably affects the critical current density at which EBIF occurs. This strongly suggests that magnetic field effects play a crucial role in instigating EBIF on the microparticles. The dependence of the value of the critical current density on the absence or presence of an ambient magnetic field cannot be accounted for by the beam-induced heating model. Consequently, this work presents robust experimental evidence suggesting that Coulomb explosion driven by electrostatic charging is the root cause of EBIF. KW - Electron beam-induced fragmentation KW - Coulomb explosion KW - X-ray diffraction KW - Lorenz transmission electron microscopy PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-600247 DO - https://doi.org/10.1016/j.ultramic.2024.113978 SN - 0304-3991 VL - 262 SP - 1 EP - 8 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-60024 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fernández, R. A1 - Cabeza, Sandra A1 - Mishurova, Tatiana A1 - Fernández-Castrillo, P. A1 - González-Doncel, G. A1 - Bruno, Giovanni T1 - Residual stress and yield strength evolution with annealing treatments in an age-hardenable aluminum alloy matrix composite JF - Materials Science & Engineering A N2 - We investigated the possibility of minimizing tensile matrix residual stresses in age hardenable aluminum alloy metal matrix composites without detrimentally affect their mechanical properties (such as yield strength). Specifically, we performed thermal treatments at different temperatures and times in an age-hardenable aluminum matrix composite 2014Al-15vol%Al2O3. Using X-ray synchrotron radiation diffraction and mechanical tests, we show that below a certain treatment temperature (250 °C) it is possible to identify an appropriate thermal treatment capable of relaxing residual stress in this composite while even increasing its yield strength, with respect to the as processed conditions. KW - Residual stress KW - X-ray diffraction KW - Annealing treatment KW - Metal matrix composite KW - Yield strength PY - 2018 DO - https://doi.org/10.1016/j.msea.2018.06.031 SN - 0921-5093 SN - 1873-4936 VL - 731 SP - 344 EP - 350 PB - Elsevier CY - Amsterdam AN - OPUS4-45255 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Heap, M.J. A1 - Lavallée, Y. A1 - Laumann, A. A1 - Hess, K.-U. A1 - Meredith, P.G. A1 - Dingwell, D.B. A1 - Huismann, Sven A1 - Weise, Frank T1 - The influence of thermal-stressing (up to 1000 °C) on the physical, mechanical, and chemical properties of siliceous-aggregate, high-strength concrete JF - Construction and building materials N2 - High-strength concrete (HSC) will experience thermal microcracking, explosive spalling, and undesirable chemical changes when exposed to high temperatures, such as during fire, engulfment by lava flow, or nuclear meltdown. Knowledge of the resultant changes in mechanical, physical, and chemical properties is paramount for hazard mitigation. We present a multidisciplinary study on the influence of thermal-stressing on HSC. Our study shows that thermal microcracking in HSC initiates at 180 °C, is more prevalent during cooling, and exhibits the Kaiser 'temperature-memory' effect. We show that residual compressive strength, indirect tensile strength, ultrasonic wave velocities, and Young’s modulus and Poisson’s ratio decrease, whilst porosity and permeability increase with increasing temperature. We discuss these data in terms of the chemical changes during thermal-stressing, provided by thermo-gravimetric analysis, differential scanning calorimetry, and X-ray diffraction, and from optical microscopic analysis of thermally-stressed samples. We provide implications for thermally-damaged HSC structures and a new method for non-destructive monitoring. KW - High strength concrete KW - Fire KW - Thermal-stressing KW - Acoustic emissions KW - Physical properties KW - Elastic moduli KW - Uniaxial compressive strength KW - Indirect tensile strength KW - Thermo-gravimetric analysis KW - X-ray diffraction PY - 2013 DO - https://doi.org/10.1016/j.conbuildmat.2013.01.020 SN - 0950-0618 VL - 42 SP - 248 EP - 265 PB - Elsevier Ltd. CY - Amsterdam AN - OPUS4-27992 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kahlau, R. A1 - Gnutzmann, Tanja A1 - Emmerling, Franziska A1 - Rademann, K. A1 - Rössler, E.A. T1 - Quinaldine: Accessing two crystalline polymorphs via the supercooled liquid JF - The journal of chemical physics N2 - Quinaldine (2-methyl quinoline) is a liquid at room temperature, which can be supercooled to reach finally the glassy state. By heating the glass above the glass transition temperature Tg = 180 K the sample performs two subsequent transitions into, likewise, dielectrically active phases. Thus, the reorientational relaxations of these phases as well as the kinetics of the phase transitions can be tracked in a highly resolved way by dielectric spectroscopy. X-ray diffraction analysis clearly shows two structurally different crystalline phases in addition to the supercooled liquid. Calorimetric measurements support the notion of first order phase transitions, occurring irreversibly in the supercooled regime, and suggest that the intermediate crystalline phase is metastable, too. Analyzing the quite distinct dielectric relaxation strengths, we discuss the possible nature of the two crystalline phases. Additionally, a very similar behavior to quinaldine is observed for 3-methyl quinoline, indicating a broad field of polymorphism among the quinoline derivatives. KW - Calorimetry KW - Dielectric liquids KW - Dielectric relaxation KW - Glass transition KW - Liquid structure KW - Organic compounds KW - Polymorphism KW - Supercooling KW - X-ray diffraction PY - 2012 DO - https://doi.org/10.1063/1.4738583 SN - 0021-9606 SN - 1089-7690 VL - 137 IS - 5 SP - 054505-1 - 054505-10 PB - American Institute of Physics CY - Melville, NY AN - OPUS4-26347 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kulla, Hannes A1 - Haferkamp, Sebastian A1 - Akhmetova, Irina A1 - Röllig, Mathias A1 - Maierhofer, Christiane A1 - Rademann, Klaus A1 - Emmerling, Franziska T1 - In situ investigations of mechanochemical one-pot syntheses JF - Angewandte Chemie International Edition N2 - We present an in situ triple coupling of synchrotron X-ray diffraction with Raman spectroscopy, and thermography to study milling reactions in real time. This combination of methods allows a correlation of the structural evolution with temperature information. The temperature information is crucial for understanding both the thermodynamics and reaction kinetics. The reaction mechanisms of three prototypical mechanochemical syntheses, a cocrystal formation, a C@C bond formation (Knoevenagel condensation), and the formation of a manganese-phosphonate, were elucidated. Trends in the temperature development during milling are identified. The heat of reaction and latent heat of crystallization of the product contribute to the overall temperature increase. A decrease in temperature occurs via release of, for example, water as a byproduct. Solid and liquid intermediates are detected. The influence of the mechanical impact could be separated from temperature effects caused by the reaction. KW - In situ studies KW - Mechanochemistry KW - Raman spectroscopy KW - Thermography KW - X-ray diffraction PY - 2018 DO - https://doi.org/10.1002/anie.201800147 SN - 1433-7851 SN - 1521-3773 VL - 57 IS - 20 SP - 5930 EP - 5933 PB - Wiley-VCH CY - Weinheim AN - OPUS4-44946 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Manzoni, Anna Maria A1 - Haas, S. A1 - Kropf, H. A1 - Duarte, J. A1 - Cakir, Cafer Tufan A1 - Dubois, F. A1 - Többens, D. A1 - Glatzel, U. T1 - Temperature evolution of lattice misfit in Hf and Mo variations of the Al 10 Co 25 Cr 8 Fe 15 Ni 36 Ti 6 compositionally complex alloy JF - Scripta Materialia N2 - Misfits of γ- γ’ based Al10Co25Cr8Fe15Ni36Ti6 and its Mo- and Hf-variations are studied up to a temperature of 980 °C and compared with Ni- and Co-based superalloys. The trace elements decrease (Hf) or increase (Mo) the edge radii of the γ’ cuboids without changing their sizes. Atom probe measurements revealed that the Hf alloy prefers the γ’ phase while Mo prefers the γ matrix, leading to a lattice parameters enhancement of both phases, as could be revealed by synchrotron X-ray diffraction. The misfit is influenced in opposite ways: Hf increases the positive misfit, while Mo reduces it at all investigated temperatures. KW - Metal and alloys KW - Transmission electron microscopy KW - X-ray diffraction KW - Atom probe tomography KW - High entropy alloy PY - 2020 DO - https://doi.org/10.1016/j.scriptamat.2020.07.013 VL - 188 SP - 74 EP - 79 PB - Elsevier Ltd. AN - OPUS4-51025 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Martin, S. A1 - Walnsch, A. A1 - Nolze, Gert A1 - Leineweber, A. A1 - Léaux, F. A1 - Scheuerlein, C. T1 - The crystal structure of (Nb0.75Cu0.25)Sn-2 in the Cu-Nb-Sn system JF - Intermetallics N2 - During the processing of superconducting Nb3Sn wire, several intermediate intermetallic phases including a previously encountered Cu-Nb-Sn phase show up. The yet unknown crystal structure of this phase is now identified by a combination of different experimental techniques and database search to be of the hexagonal NiMg2 type with a proposed composition of about (Nb0.75Cu0.25)Sn2. The structure determination started from an evaluation of the lattice parameters from EBSD Kikuchi patterns from quenched material suggesting hexagonal or orthorhombic symmetry. A database search then led to the hexagonal NiMg2 type structure, the presence of which was confirmed by a Rietveld analysis on the basis of high energy synchrotron X-ray powder diffraction data. Assuming a partial substitution of Nb in orthorhombic NbSn2 by Cu, the change of the valence electron concentration provokes a structural transformation from the CuMg2 type for NbSn2 to the NiMg2 type for (Nb0.75Cu0.25)Sn2. In the previous literature the (Nb0.75Cu0.25)Sn2 phase described here has occasionally been referred to as Nausite. KW - Electron backscatter diffraction KW - X-ray diffraction KW - Intermetallic compound KW - Structure solution KW - Superconductor PY - 2017 DO - https://doi.org/10.1016/j.intermet.2016.09.008 SN - 0966-9795 SN - 1879-0216 VL - 80 SP - 16 EP - 21 PB - Elsevier Ltd. AN - OPUS4-37874 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Matos, P. R. de A1 - Andrade Neto, J. S. A1 - Durlo Tambara, Luis Urbano A1 - Rodríguez, E. D. A1 - Kirchheim, A. P. A1 - Campos, C. E. M. de T1 - Measuring the early-age volumetric change of cement paste through in-situ XRD JF - Materials Today Communications N2 - Volumetric changes follow Portland cement hydration reactions: aluminates' hydration is generally expansive, whereas silicates' reaction leads to shrinkage. Determining the volumetric variation at very early ages (i.e., first minutes/hours) presents operational challenges; most standards prescribe the measurement on specimens that are already hardened, while measurements from the fresh state are not standardized. This article reports the first attempt to use in-situ X-ray diffraction (XRD) to measure the early-age volumetric variation of a cementitious paste. For this purpose, a C3A + gypsum paste was assessed for 36 h, measuring its vertical displacement over time through XRD. The results showed that the expansion increased in the first ∼13 h, in line with the ettringite formed up to ∼11 h. In addition, the volumetric expansion agreed well with the heat release in calorimetry. It is concluded that the volumetric variation measurement of cementitious pastes through in-situ XRD is a promising technique, but further studies are needed to make this technique consolidated. KW - X-ray diffraction KW - Shrinkage KW - Expansion KW - Hydration KW - Portland cement PY - 2023 DO - https://doi.org/10.1016/j.mtcomm.2023.106857 SN - 2352-4928 VL - 36 SP - 1 EP - 4 PB - Elsevier Ltd. CY - Amsterdam AN - OPUS4-58107 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mishurova, Tatiana A1 - Bruno, Giovanni A1 - Evsevleev, Sergei A1 - Sevostianov, I. T1 - Determination of macroscopic stress from diffraction experiments: A critical discussion JF - Journal of Applied Physics N2 - The paper is motivated by some inconsistencies and contradictions present in the literature on the calculation of the so-called diffraction elastic constants. In an attempt at unifying the views that the two communities of Materials Science and Mechanics of Materials have on the subject, we revisit and define the terminology used in the field. We also clarify the limitations of the commonly used approaches and Show that a unified methodology is also applicable to textured materials with a nearly arbitrary grain shape. We finally compare the predictions based on this methodology with experimental data obtained by in situ synchrotron radiation diffraction on additively manufactured Ti-6Al4V alloy. We show that (a) the transverse isotropy of the material yields good agreement between the best-fit isotropy approximation (equivalent to the classic Kröner’s model) and the experimental data and (b) the use of a general framework allows the calculation of all components of the tensor of diffraction elastic constants, which are not easily measurable by diffraction methods. This allows us to extend the current state-of-the-art with a predictive tool. KW - Additive manufacturing KW - X-ray diffraction KW - Elastic constants KW - Stress concentration tensor PY - 2020 DO - https://doi.org/10.1063/5.0009101 VL - 128 IS - 2 SP - 025103 PB - AIP Publishing AN - OPUS4-50993 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Müller, Bernd R. T1 - Synchrotronstrahlung: verbesserte Refraktions- und Absorptions-Mikro-CT für die zerstörungsfreie Materialcharakterisierung JF - ZfP-Zeitung N2 - Röntgenstrahlung eignet sich besonders gut zur zerstörungsfreien Charakterisierung von Werkstoffen. Mit ihrer Hilfe lassen sich z.B. Risse und Poren in Werkstoffen erkennen. Die Risserkennbarkeit ist jedoch von der Rissgröße relativ zum Auflösungsvermögen des Detektors abhängig. Risse, Poren oder Einschlüsse können in Radiogrammen nur dann erkannt werden, wenn sie größer sind als das Detektorelement, das die Röntgenstrahlen registriert. Das hier vorgestellte neuartige Synchrotron-Refraktions-Computer-Tomographie-Verfahren ist jedoch in der Lage, auch Risse zu erkennen, deren Größe weit unterhalb des Auflösungsvermögens des Detektors liegt. Das Verfahren basiert auf dem bisher wenig genutzten Phänomen der Brechung von Röntgenstrahlen an den inneren Grenzflächen mikroskopisch strukturierter Objekte. Durch den Vergleich zwischen absorptionsbasierter und refraktionsbasierter Computer Tomographie Untersuchungen mit Synchrotronstrahlung an einer geschädigten Faserverbundprobe wird das Potenzial der Synchrotron-Refraktions-Computer-Tomographie demonstriert. KW - Synchrotronstrahlung KW - Refraktion KW - Diffraktion KW - Kleinwinkelstreuung KW - Materialcharakterisierung KW - Zerstörungsfrei KW - Synchrotron radiation KW - X-ray diffraction KW - Small angle scattering KW - Materials characterization KW - Non-destructive PY - 2015 SN - 1616-069X SN - 0948-5112 VL - 146 SP - 46 EP - 51 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung CY - Berlin AN - OPUS4-34305 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Quillard, S. A1 - Paris, M. A1 - Deniard, P. A1 - Gildenhaar, Renate A1 - Berger, Georg A1 - Obadia, L. A1 - Bouler, J.-M. T1 - Structural and spectroscopic characterization of a series of potassium- and/or sodium-substituted beta-tricalcium phosphate JF - Acta biomaterialia N2 - In this paper, we report X-ray diffraction investigations as well as Raman and solid-state 31P and 23Na magic angle spinning nuclear magnetic resonance (NMR) characterization of three series of calcium orthophosphates. The general formulae of the studied compounds are Ca10.5-x/2Mx(PO4)7, where M = K or Na and x = 0, 0.25, 0.50, 0.75, 1.0; and Ca10KxNa1-x(PO4)7, where x = 0, 0.25, 0.5, 0.75, 1.0. These calcium orthophosphates are found to be isostructural with β-tricalcium phosphate (β-TCP, Ca3(PO4)2) with the substitution of some calcium sites by potassium and/or sodium cations. The unit cell parameters vary continuously with the level of substitution, a characteristic of these solid solutions. The Raman spectra show the different vibrational bands of the phosphate groups PO4, while the NMR chemical shifts are sensitive to the non-equivalent phosphorus and sodium ions present in these substituted samples. As both Raman and NMR spectroscopies are local probes, they offer tools to distinguish between these different phosphorus and phosphate groups, according to their structural site and local environment, especially the type of cation substituent. A convenient decomposition of the Raman and NMR spectra into Gaussian–Lorentzian components leads us to propose an assignment of the main observed bands of these substituted β-TCPs. KW - Bioceramics KW - Tricalcium phosphate KW - X-ray diffraction KW - Raman spectroscopy KW - Solid-state NMR spectroscopy PY - 2011 DO - https://doi.org/10.1016/j.actbio.2010.12.016 SN - 1742-7061 VL - 7 IS - 4 SP - 1844 EP - 1852 PB - Elsevier CY - Amsterdam AN - OPUS4-23405 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rautenberg, Max A1 - Bhattacharya, Biswajit A1 - Akhmetova, Irinia A1 - Emmerling, Franziska T1 - Mechanochemical and solution syntheses of two novel cocrystals of orcinol with two N,N0-Dipyridines: Structural diversity with varying ligand flexibility JF - Journal of Molecular Structure N2 - We studied the influence of coformers flexibility on the supramolecular assembly of 5-substituted resorcinol. Two cocrystals of orcinol (ORL) with two dipyridine molecules, i.e. 1,2-di(4-pyridyl)ethane (ORLeBPE) and 1,2-di(4-pyridyl)ethylene (ORLeBPY), were prepared by mechanochemical synthesis and slow evaporation of solvent. The new crystalline solids were thoroughly characterized by single crystal Xray diffraction (SCXRD), powder X-ray diffraction analysis (PXRD), Fourier-transform infrared spectroscopy (FT-IR), differential thermal analysis (DTA), and thermogravimetric analysis (TGA). Structural determination reveals that in both cocrystals, the phenolepyridine, i.e. OeH/N(py) heterosynthon takes the main role in the formation of cocrystals. In ORLeBPE, the components form infinite 1D zig-zag chains, which are extended to 2D layer structure by inter-chain CeH/O interactions between BPE hydrogen atoms and hydroxyl oxygen atoms of ORL. In ORLeBPY, the components form a 0D fourcomponent complex. Formation of the discrete assemblies is attributed to the comparative rigid nature of BPY, which restricts the formation of an extended network. KW - Cocrystal KW - Single crystal KW - X-ray diffraction KW - Mechanochemistry PY - 2020 DO - https://doi.org/10.1016/j.molstruc.2020.128303 SN - 0022-2860 VL - 1217 SP - 128303 PB - Elsevier B.V. AN - OPUS4-51023 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sarfraz, Adnan A1 - Simo, A. A1 - Fenger, R. A1 - Christen, W. A1 - Rademann, K. A1 - Panne, Ulrich A1 - Emmerling, Franziska T1 - Morphological diversity of caffeine on surfaces: needles and hexagons JF - Crystal growth & design N2 - A systematic crystal morphology study on the pharmaceutical model compound caffeine has been conducted on different surfaces: silicon, silver, soda lime glass, and silver subsurface ion-exchanged soda-lime silicate (SIMO) glasses. The morphology of the solid caffeine deposits has been investigated using environmental scanning electron microscopy (ESEM), atomic force microscopy (AFM), and X-ray diffraction (XRD). Needle-shaped caffeine crystals have been observed by drop-casting and also by applying the rapid expansion of supercritical solutions (RESS) technique using supercritical carbon dioxide. The aspect ratio of the crystalline needles typically vary between 10 and 100, but have been observed as large as 500. The XRD data of the RESS products indicate unambiguously the presence of the thermodynamically most stable polymorph of caffeine known as the β-form. Under defined conditions we observe a unique, surface-mediated morphology for caffeine crystals with nearly perfect hexagonal shape. The relative fraction of the hexagons was seen to strongly increase especially when SIMO glasses were used. These hexagons have a distinct upper size limit depending on the solvent and substrate being used. The size distribution analysis of the hexagons yielded an average perimeter of typically 10 µm. The mechanism of the formation process of this new hexagonal motif is explained in terms of the spinodal dewetting of the thin film of caffeine solution on the surface. KW - Caffeine KW - Silicon KW - Silver KW - Ion exchanged soda lime silicate glass KW - ESEM KW - AFM KW - X-ray diffraction KW - RESS KW - Carbon dioxide KW - Supercritical fluids PY - 2012 DO - https://doi.org/10.1021/cg101358q SN - 1528-7483 VL - 12 IS - 2 SP - 583 EP - 588 PB - American Chemical Society CY - Washington, DC, USA AN - OPUS4-25457 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Scheuerlein, C. A1 - Andrieux, J. A1 - Michels, M. A1 - Lackner, F. A1 - Chiriac, R. A1 - Hagner, M. A1 - Di Michiel, M. A1 - Meyer, Christian A1 - Toche, F. ED - Foley, C. P. T1 - Effect of the fabrication route on the phase and volume changes during the reaction heat treatment of Nb3Sn superconducting wires JF - Superconductor Science and Technology N2 - Accelerator magnets that can reach magnetic fields well beyond the Nb-Ti performance limits are presently being built and developed, using Nb3Sn superconductors. This technology requires reaction heat treatment (RHT) of the magnet coils, during which Nb3Sn is formed from its ductile precursor materials (a “wind and react” approach). The Nb3Sn microstructure and microchemistry are strongly influenced by the conductor fabrication route, and by the Phase changes during RHT. By combining in situ differential scanning calorimetry, high Energy synchrotron x-ray diffraction, and micro-tomography experiments, we have acquired a unique data set that describes in great detail the phase and microstructure changes that take place during the processing of restacked rod process (RRP), powder-in-tube (PIT), and internal tin (IT) Nb3Sn wires. At temperatures below 450 ° the phase evolutions in the three wire types are similar, with respectively solid state interdiffusion of Cu and Sn, Cu6Sn5 formation, and Cu6Sn5 peritectic transformation. Distinct differences in phase evolutions in the wires are found when temperatures exceed 450 °C. The volume changes of the conductor during RHT are a difficulty in the production of Nb3Sn accelerator magnets. We compare the wire diameter changes measured in situ by dilatometry with the phase and void volume evolution of the three types of Nb3Sn wire. Unlike the Nb3Sn wire length changes, the wire diameter evolution is characteristic for each Nb3Sn wire type. The strongest volume increase, of about 5%, is observed in the RRP wire, where the main diameter increase occurs above 600 °C upon Nb3Sn formation. KW - Nb3Sn KW - Microstructure KW - Phase transformations KW - Volume changes KW - X-ray diffraction KW - Differential scanning calorimetry KW - Synchrotron micro-tomography PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-505128 DO - https://doi.org/10.1088/1361-6668/ab627c VL - 33 IS - 3 SP - 034004 PB - IOP Publishing CY - Bristol (UK) AN - OPUS4-50512 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schlegel, Moritz-Caspar A1 - Sarfraz, Adnan A1 - Müller, Urs A1 - Panne, Ulrich A1 - Emmerling, Franziska T1 - First seconds in a building's life - In situ synchrotron X-ray diffraction study of cement hydration on the millisecond timescale JF - Angewandte Chemie / International Edition N2 - Setting cement: Highly dynamic hydration processes that occur during the first seconds of cement hydration were studied by time-resolved synchrotron X-ray diffraction. Polycarboxylate ether additives were found to influence the formation of the initial crystalline hydration products on a molecular level. KW - Cement hydration KW - Colloidal suspensions KW - In situ analysis KW - X-ray diffraction KW - SyXRD KW - High resolution KW - In-situ PY - 2012 DO - https://doi.org/10.1002/anie.201200993 SN - 1433-7851 SN - 1521-3773 SN - 0570-0833 VL - 51 IS - 20 SP - 4993 EP - 4996 PB - Wiley-VCH CY - Weinheim AN - OPUS4-26287 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schlegel, Moritz-Caspar A1 - Többens, D. A1 - Svetogorov, R. A1 - Krüger, M. A1 - Stock, N. A1 - Reinsch, H. A1 - Wallacher, D. A1 - Stewart, R. A1 - Russina, M. T1 - Conformation-controlled hydrogen storage in the CAU-1 metal-organic framework JF - Physical Chemistry Chemical Physics N2 - We have studied the mechanism of hydrogen storage in the aluminium based metal–organic framework CAU-1 or [Al4(OH)2 OCH3)4(O2C-C6H3NH2-CO2)3] using a complementary multidisciplinary approach of volumetric gas sorption analysis, in situ neutron diffraction and spectroscopy and ab initio calculations. The structure of CAU-1 forms two different types of microporous cages: (i) an octahedral cage with a diameter of about 10 Å and (ii) a tetrahedral cage with a diameter of about 5 Å. Though all metal sites of CAU-1 are fully coordinated, the material exhibits relatively high storage capacities, reaching 4 wt% at a temperature of 70 K. Our results reveal that hydrogen sorption is dominantly driven by cooperative guest–guest interactions and interactions between guest hydrogen molecules and organic linkers. The adsorption of hydrogen on the organic linkers leads to the contraction of the host framework structure and as a result to changes in the electronic potential surface inside the pores. This, in turn, leads to cooperative rearrangement of the molecules inside the pores and to the formation of additionally occupied positions, increasing hydrogen uptake. At the final stage we observe the formation of solid amorphous hydrogen inside the pores. KW - Hydrogen storage KW - MOF KW - X-ray diffraction KW - Neutron diffraction KW - Neutron scattering PY - 2016 DO - https://doi.org/10.1039/c6cp05310f SN - 1463-9076 SN - 1463-9084 VL - 18 SP - 29258 EP - 29267 PB - The Royal Soc. of Chemistry CY - Cambridge AN - OPUS4-37794 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schraut, Katharina A1 - Adamczyk, Burkart A1 - Adam, Christian A1 - Stephan, D. A1 - Meng, Birgit A1 - Simon, Sebastian A1 - von Werder, Julia T1 - Synthesis and characterisation of alites from reduced basic oxygen furnace slags JF - Cement and Concrete Research N2 - Basic oxygen furnace slags (BOFS) are by-products of the steelmaking process. Several researchers have studied the production of Portland cement clinker and metallic iron from BOFS via a reductive treatment. In this study, we applied a carbothermal reduction of BOFS in a technical-scale electric arc furnace and characterised the clinker-like products. Those clinker-like non-metallic products (NMPs) had a chemical and mineralogical composition comparable to clinker for ordinary Portland cement (OPC) and contained large elongated alite crystals as major component. The pure NMPs reacted more slowly and achieved a lower degree of hydration compared with commercial OPC. If the reactivity of the products can be further increased by employing specific adaptations, it can be used as a full clinker substitute for OPC. Nevertheless, it is also an option to use the material without further modifications as a cement component or concrete addition, which contributes to the strength development in both cases. KW - BOFS KW - Hydration products KW - Thermal analysis KW - X-ray diffraction PY - 2021 DO - https://doi.org/10.1016/j.cemconres.2021.106518 SN - 0008-8846 VL - 147 SP - 6518 PB - Elsevier Ltd. AN - OPUS4-52939 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schubert, G. A1 - Reck, Günter A1 - Jancke, Harald A1 - Kraus, Werner A1 - Patzelt, C. T1 - Uric acid monohydrate - a new urinary calculus phase JF - Urological research N2 - In our laboratory more than 100,000 urinary calculi have been analysed since 1972. Amongst this huge sample, 15 specimens originating from a total of eight patients were observed showing similar characteristics but escaping unambiguous identification with any of the substances that have been described so far in urinary concrements. Therefore, the unknown substance was submitted to a more extended analytical regimen. Structural analysis by x-ray crystallography turned out to be most successful, identifying the unknown material as uric acid monohydrate. Uric acid monohydrate crystallizes in the monocline space group P21/c. Within the crystal, uric acid and water molecules form continuous layers by hydrogen bonds. This is in contrast to uric acid in its water free and its dihydrate forms, which both crystallize by forming 3-dimensional networks To the best of our knowledge , the existence of a monohydrate form of uric acid has not been reported so far. Accordingly, this is the first report on uric acid monohydrate as a urinary stone component. The frequency of only 0.015% in our survey indicates that uric acid monohydrate is rarely the main component in concrements, in contrast to uric acid and uric acid dihydrate with frequencies of 10% and 6%, respectively. The infrared spectrum of uric acid monohydrate is very similar to that of the other crystal forms of uric acid. Because of this similarity and its low frequency, uric acid monohydrate may have been overlooked as a component of urinary concrements. X-ray diffraction allows for better differentiation in routine stone analysis. All samples of uric acid monohydrate were found by solid state NMR spectroscopy to be highly contaminated by amorphous material. This material consisted of long aliphatic chains reminiscent of lipids and fatty acids, respectively. Concrements consisting of other forms of uric acid or urate lacked this amorphous component. Therefore, a role of this aliphatic material has to be taken into consideration when discussing the conditions that may favour the rare formation of concrements from uric acid monohydrate. As for as the metabolic situation of the affected patients is concerned, no common peculiarities became evident by a retrospective survey. KW - Uric acid monohydrate KW - Urinary calculus KW - Crystal structure KW - Solid state NMR KW - X-ray diffraction KW - Infrared spectroscopy PY - 2005 DO - https://doi.org/10.1007/s00240-005-0467-5 SN - 0300-5623 SN - 1434-0879 VL - 33 IS - 3 SP - 231 EP - 238 PB - Springer CY - Berlin AN - OPUS4-7676 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schumacher, G. A1 - Darowski, N. A1 - Zizak, I. A1 - Klingelhöffer, Hellmuth A1 - Neumann, W. T1 - Two-stage relaxation of damage structure in strongly creep-deformed single crystal superalloy SC16 measured by means of X-ray diffraction JF - Scripta materialia KW - Superalloys KW - SC16 KW - Creep-deformation KW - Relaxation KW - X-ray diffraction PY - 2009 DO - https://doi.org/10.1016/j.scriptamat.2008.09.009 SN - 1359-6462 SN - 1872-8456 VL - 60 IS - 2 SP - 88 EP - 91 PB - Elsevier CY - Oxford AN - OPUS4-18304 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Steckenmesser, D. A1 - Vogel, Christian A1 - Herzel, Hannes A1 - Félix, R. A1 - Adam, Christian A1 - Steffens, D. T1 - Thermal treatment of sewage sludge for phosphorus fertilizer production: a model experiment JF - Journal of Plant Nutrition N2 - Phosphorus (P) resource availability and quality is declining and recycling P-fertilizers from waste materials are becoming increasingly important. One important secondary P resource is sewage sludge (SSL) where P is often bound as aluminum phosphate (Al-P), iron phosphate (Fe-P) and polyphosphate (poly-P), respectively. Thermal treatment in different ways is a promising way in P recycling to produce highly plant-available P-fertilizers. To investigate mechanisms behind transformation of hardly available P-species toward plant-available P forms we treated a model SSL containing different kinds of defined P sources by low-temperature conversion (LTC) at 500 °C and subsequent thermochemical treatment of the LTC product with Na additives (TCT) at 950 °C, respectively. Pot experiments with ryegrass were carried out to determine the plant availability of P of the different treatments. The poly-P (here pyrophosphates) based fertilizers had a very high plant availability after both thermal treatments. During LTC treatment the plant availability of the Fe-P and Al-P variants increased because of the Formation of Fe(II) phosphates and/or pyro-/polyphosphates. Especially the formation of Al-polyphosphate shows a high plant availability. The subsequent TCT further increased strongly the plant availability of the Fe-P variants because of the formation of highly plant-available CaNaPO4. Thus, a direct TCT without prior LTC probably also produce CaNaPO4 and is recommended for Fe-P based SSL. However, a molar Ca/P ratio of � 1 in the fertilizer is favorable for CaNaPO4 formation. Thus, the knowledge on the source of primary P in SSL is essential for choosing the accurate thermal treatment method to produce highly plant-available P-fertilizers from SSL. KW - Phosphorus KW - Sewage sludge KW - X-ray diffraction KW - X-ray absorption near-edge structure (XANES) spectroscopy KW - Fertilizer PY - 2021 DO - https://doi.org/10.1080/01904167.2021.1994595 SN - 0190-4167 VL - 45 IS - 8 SP - 1123 EP - 1133 PB - Taylor & Francis Online AN - OPUS4-53755 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stroh, Julia A1 - Feiler, Torvid A1 - Ali, N. Z. A1 - Minas da Piedade, M. E. A1 - Emmerling, Franziska T1 - Mechanistic Insights into a Sustainable Mechanochemical Synthesis of Ettringite JF - ChemistryOpen N2 - Mechanochemistry offers an environmentally benign and facile synthesis method for a variety of cement paste constituents. In addition, these methods can be used to selectively tune the properties of cement components. The mineral ettringite is an important component of cementitious materials and has additional technological potential due to its ion exchange properties. Synthesis of ettringite via mechanochemistry is an environmentally friendly alternative to conventional wet-chemical synthesis established in industry. This contribution explores the mechanism of a two-step mechanochemical synthesis of ettringite, which was previously found to greatly improve the reaction conversion as compared with one-pot synthesis. The crystallinity of Al(OH)3 was found to decrease during the first stage of this mechanochemical synthesis. This was correlated to a significant decrease in the particle size of Al(OH)3 in this stage. No other significant changes were found for the other components, suggesting that mechanochemical activation of Al(OH)3 is responsible for the enhanced formation of ettringite by the two-step approach. The environmentally friendly approach developed for ettringite synthesis offers a versatile synthetic strategy, which can be applied to synthesise further cementitious materials. KW - Ettringite KW - Mechanochemistry KW - Sustainability KW - X-ray diffraction PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-489172 DO - https://doi.org/10.1002/open.201900215 VL - 8 IS - 7 SP - 1012 EP - 1019 PB - ChemPubSoc AN - OPUS4-48917 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Suárez Ocaño, Patricia A1 - Manzoni, Anna Maria A1 - Lopez-Galilea, I. A1 - Ruttert, B. A1 - Laplanche, G. A1 - Agudo Jácome, Leonardo T1 - Influence of cooling rate on the microstructure and room temperature mechanical properties in the refractory AlMo0.5NbTa0.5TiZr superalloy JF - Journal of Alloys and Compounds N2 - Refractory chemically complex alloys with bcc-based microstructures show great potential for high-temperature applications but most of them exhibit limited room-temperature ductility, which remains a challenge. One such example is the AlMo0.5NbTa0.5TiZr alloy, mainly consisting of a nano-scaled structure with an ordered B2 matrix and a high-volume fraction of aligned cuboidal and coherently embedded A2 precipitates. This work aims to investigate how the cooling rate after hot isostatic pressing of the AlMo0.5NbTa0.5TiZr alloy affects its microstructure and its resulting hardness and fracture toughness at room temperature. A slow cooling rate of 5 °C/min leads to a coarse microstructure consisting of aligned slabs (mean A2 precipitate ≈ 25 nm) with a nanohardness of about 8 GPa. In contrast, after the fastest cooling rate (30 °C/min), the A2 precipitates become more cubic with an edge length of ≈ 16 nm, resulting in an increase in nanohardness by 10 %. The fracture toughness is roughly independent of the cooling rate and its mean value (≈ 4.2 MPa∙m1/2) resembles that of some B2 intermetallics and other A2/B2 alloys. As the lattice misfit between the A2 and B2 phases is known to play a key role in microstructure formation and evolution, its temperature dependence between 20 and 900 °C was investigated. These findings offer insights into the evolution of the microstructure and room-temperature mechanical properties of the AlMo0.5NbTa0.5TiZr alloy, which could help the development of advanced chemically complex alloys. KW - High entropy alloy KW - Lattice misfit KW - Scanning electron microscopy KW - Transmission electron microscopy KW - X-ray diffraction KW - Refractory alloy PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-572809 DO - https://doi.org/10.1016/j.jallcom.2023.169871 SN - 0925-8388 VL - 949 SP - 169871 PB - Elsevier B.V. AN - OPUS4-57280 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Varin, R.A. A1 - Czujko, T. A1 - Chiu, C. A1 - Pulz, Robert A1 - Wronski, Z. S. T1 - Synthesis of nanocomposite hydrides for solid-state hydrogen storage by controlled mechanical milling techniques JF - Journal of alloys and compounds KW - Hydrogen storage materials KW - Nanocomposite hydrides KW - Rule-of-mixtures KW - Mechanical milling KW - X-ray diffraction KW - Differential scanning calorimetry PY - 2009 DO - https://doi.org/10.1016/j.jallcom.2008.07.207 SN - 0925-8388 SN - 1873-4669 VL - 483 IS - 1-2 SP - 252 EP - 255 PB - Elsevier Sequoia CY - Lausanne AN - OPUS4-20282 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Winterlik, J. A1 - Fecher, G.H. A1 - Jenkins, C.A. A1 - Medvedev, S. A1 - Felser, C. A1 - Kübler, J. A1 - Mühle, C. A1 - Doll, K. A1 - Jansen, M. A1 - Palasyuk, T. A1 - Trojan, I. A1 - Eremets, M.I. A1 - Emmerling, Franziska T1 - Exotic magnetism in the alkali sesquioxides Rb4O6 and Cs4O6 JF - Physical review B KW - Caesium compounds KW - Crystal structure KW - Density functional theory KW - Electronic structure KW - Ferromagnetic materials KW - Frustration KW - Magnetic transitions KW - Magnetisation KW - Raman spectra KW - Rubidium compounds KW - Spin glasses KW - X-ray diffraction PY - 2009 DO - https://doi.org/10.1103/PhysRevB.79.214410 SN - 1098-0121 SN - 0163-1829 SN - 0556-2805 SN - 1095-3795 SN - 1550-235X VL - 79 IS - 21 SP - 214410-1 - 214410-6 PB - American Institute of Physics CY - Melville, NY AN - OPUS4-19796 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Yesilcicek, Yasemin A1 - Haas, S. A1 - Suárez Ocano, Patricia A1 - Zaiser, E. A1 - Hesse, René A1 - Többens, D. M. A1 - Glatzel, U. A1 - Manzoni, Anna Maria T1 - Controlling Lattice Misfit and Creep Rate Through the γ' Cube Shapes in the Al10Co25Cr8Fe15Ni36Ti6 Compositionally Complex Alloy with Hf and W Additions JF - High Entropy Alloys & Materials N2 - Trace elements play an important role in the fine-tuning of complex material properties. This study focuses on the correlation of microstructure, lattice misfit and creep properties. The compositionally complex alloy Al10Co25Cr8Fe15Ni36Ti6 (in at. %) was tuned with high melting trace elements Hf and W. The microstructure consists of a γ matrix, γ' precipitates and the Heusler phase and it is accompanied by good mechanical properties for high temperature applications. The addition of 0.5 at.% Hf to the Al10Co25Cr8Fe15Ni36Ti6 alloy resulted in more sharp-edged cubic γ′ precipitates and an increase in the Heusler phase amount. The addition of 1 at.% W led to more rounded γ′ precipitates and the dissolution of the Heusler phase. The shapes of the γ' precipitates of the alloys Al9.25Co25Cr8Fe15Ni36Ti6Hf0.25W0.5 and Al9.25Co25Cr8Fe15Ni36Ti6Hf0.5W0.25, that are the alloys of interest in this paper, create a transition from the well-rounded precipitates in the alloy with 1% W containing alloy to the sharp angular particles in the alloy with 0.5% Hf. While the lattice misfit has a direct correlation to the γ' precipitates shape, the creep rate is also related to the amount of the Heusler phase. The lattice misfit increases with decreasing corner radius of the γ' precipitates. So does the creep rate, but it also increases with the amount of Heusler phase. The microstructures were investigated by SEM and TEM, the lattice misfit was calculated from the lattice parameters obtained by synchrotron radiation measurements. KW - High entropy alloy KW - Lattice misfit KW - Creep KW - Transmission electron microscopy KW - X-ray diffraction PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-565655 DO - https://doi.org/10.1007/s44210-022-00009-1 SP - 1 EP - 9 PB - Springer AN - OPUS4-56565 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 JF - Zeitschrift für anorganische und allgemeine Chemie 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 - Österle, Werner A1 - Orts Gil, Guillermo A1 - Gross, Thomas A1 - Deutsch, Cornelius A1 - Hinrichs, R. A1 - Vasconcellos, M.A.Z. A1 - Zoz, H. A1 - Yigit, D. A1 - Sun, X. T1 - Impact of high energy ball milling on the nanostructure of magnetite-graphite and magnetite-graphite-molybdenum disulphide blends JF - Materials characterization N2 - Different, partly complementary and partly redundant characterization methods were applied to study the transition of magnetite, graphite and MoS2 powders to mechanically alloyed nanostructures. The applied methods were: Transmission electron microscopy (TEM), Mössbauer spectroscopy (MS), Raman spectroscopy (RS), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). The main objective was to prepare a model material providing the essential features of a typical tribofilm forming during automotive braking, and to assess the impact of different constituents on sliding behaviour and friction level. Irrespective of the initial grain size, the raw materials were transferred to a nanocrystalline structure and mixed on a nanoscopic scale during high energy ball milling. Whereas magnetite remained almost unchanged, graphite and molybdenum disulphide were transformed to a nanocrystalline and highly disordered structure. The observed increase of the coefficient of friction was attributed to a loss of lubricity of the latter ingredient due to this transformation and subsequent oxidation. KW - Ball milling KW - Mössbauer spectroscopy KW - Raman spectroscopy KW - Transmission electron microscopy KW - X-ray diffraction KW - X-ray photoelectron spectroscopy PY - 2013 DO - https://doi.org/10.1016/j.matchar.2013.09.007 SN - 1044-5803 SN - 1873-4189 VL - 86 SP - 28 EP - 38 PB - Elsevier Inc. CY - New York, NY AN - OPUS4-29697 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Österle, Werner A1 - Rooch, Heidemarie A1 - Pyzalla, A. A1 - Wang, L. T1 - Investigation of white etching layers on rails by optical microscopy, electron microscopy, X-ray and synchrotron X-ray diffraction JF - Materials science and engineering A N2 - Patches of white etching layers on rail surfaces were investigated using sophisticated techniques like cross-sectional transmission electron microscopy (XTEM) and synchroton X-ray diffraction. Optical microscopy failed to resolve the microstructure, but in the TEM submicron grains with high dislocation densities and occasional twins, which are characteristic features of high carbon martensite, were observed. The martensitic structure was confirmed by evaluation of synchroton X-ray diffraction line profiles. The latter technique also allowed to determine dislocation densities of the order of 1012 cm-2 and residual compressive stresses of about 200 MPa. KW - Cross-sectional transmission electron microscopy KW - White etching layers KW - X-ray diffraction PY - 2001 DO - https://doi.org/10.1016/S0921-5093(00)01842-6 SN - 0921-5093 SN - 1873-4936 VL - 303 SP - 150 EP - 157 PB - Elsevier CY - Amsterdam AN - OPUS4-2370 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -