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 -