TY - JOUR A1 - Leiterer, Jork A1 - Leitenberger, W. A1 - Emmerling, Franziska A1 - Thünemann, Andreas A1 - Panne, Ulrich T1 - The use of an acoustic levitator to follow crystallization in small droplets by energy-dispersive X-ray diffraction N2 - For the investigation of small sample volumes, the use of an acoustic levitator was tested as a `sample holder' for hovering droplets in a synchrotron beam. It might be advantageous to use levitated droplets instead of samples confined in solid holders, especially for the study of crystallization processes where the influence of containing walls has to be minimized. In a first experiment, the crystallization of sodium chloride in a small droplet of aqueous solution has been followed with a time resolution of 30 s. The collected diffraction peaks are compared with data in the ICSD database. KW - EDXD KW - Noncontact measurement technique KW - X-ray-scattering KW - Synchrotron-radiation KW - Acoustic levitation PY - 2006 U6 - https://doi.org/10.1107/S0021889806024915 SN - 0021-8898 SN - 1600-5767 VL - 39 IS - 5 SP - 771 EP - 773 PB - Blackwell CY - Oxford AN - OPUS4-13516 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schlegel, Moritz-Caspar A1 - Müller, Urs A1 - Panne, Ulrich A1 - Emmerling, Franziska A1 - Meng, Birgit ED - Rogge, A. ED - Meng, B. T1 - Neue Wege in der Zementanalytik - Hochaufgelöste in-situ Sy-XRD T2 - 52. DAfStb-Forschungskolloquium CY - Berlin, Deutschland DA - 2011-11-07 PY - 2011 SN - 978-3-9814281-0-0 SP - 18 EP - 24 PB - BAM Bundesanstalt für Materialforschung und -prüfung CY - Berlin AN - OPUS4-25197 LA - deu 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 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 U6 - 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 - Schlegel, Moritz-Caspar A1 - Wenzel, Klaus-Jürgen A1 - Sarfraz, Adnan A1 - Panne, Ulrich A1 - Emmerling, Franziska T1 - A wall-free climate unit for acoustic levitators N2 - Acoustic levitation represents the physical background of trapping a sample in a standing acoustic wave with no contact to the wave generating device. For the last three decades, sample holders based on this effect have been commonly used for contact free handling of samples coupled with a number of analytical techniques. In this study, a wall-free climate unit is presented, which allows the control of the environmental conditions of suspended samples. The insulation is based on a continuous cold/hot gas flow around the sample and thus does not require any additional isolation material. This provides a direct access to the levitated sample and circumvents any influence of the climate unit material to the running analyses. KW - Acoustic levition PY - 2012 U6 - https://doi.org/10.1063/1.4705968 SN - 0034-6748 SN - 1089-7623 VL - 83 IS - 5 SP - 055101-1 - 055101-3 PB - American Institute of Physics CY - Melville, NY AN - OPUS4-25881 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 - Erste Sekunden im Leben eines Bauwerks - In-situ-Synchrotron-Röntgenbeugungsuntersuchungen der Zementhydratation mit Millisekunden-Auflösung N2 - Höchst dynamische Hydratationsprozesse in den ersten Sekunden bei der Entstehung eines Bauwerkes lassen sich mithilfe von Synchrotron-Röntgenbeugung mit einer sehr hohen Zeitauflösung nachverfolgen. Der Schwerpunkt lag dabei auf der Beeinflussung der Bildung erster kristalliner Hydratationsprodukte während des Frühstadiums der Zementhydratation. KW - SyXRD KW - High resolution KW - In-situ KW - Colloidal suspension KW - Cement hydration KW - In-situ-Analyse KW - Kolloidale Suspensionen KW - Röntgenbeugung KW - Zementhydratation PY - 2012 U6 - https://doi.org/10.1002/ange.201200993 SN - 0044-8249 SN - 0932-2140 SN - 1521-3757 VL - 124 IS - 20 SP - 5078 EP - 5081 PB - Wiley-VCH CY - Weinheim AN - OPUS4-26284 LA - deu 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 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 U6 - 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 - Leiterer, Jork A1 - Emmerling, Franziska A1 - Panne, Ulrich A1 - Christen, W. A1 - Rademann, K. T1 - Tracing Coffee Tabletop Traces N2 - Crystallization processes under different conditions are of fundamental interest in chemistry, pharmacy, and medicine. Therefore, we have studied the formation of micro- and nanosized crystals using water-caffeine (1,3,7-trimethyl-1H-purine-2,6(3H,7H)-dione) solutions under ambient conditions as a relevant model system. When droplets of an aqueous caffeine solution evaporate and eventually dry on surfaces (glass, polystyrene, and polyester), stable “coffee tabletop” rings with a perimeter of typically 3 mm are formed after 20 to 50 min. Using a micro focus X-ray beam available at the BESSY µSpot-beamline, the fine structure of different caffeine needles can be distinguished. Unexpectedly, both crystal modifications (α- and β-caffeine) are present, but locally separated in these rings. Furthermore, AFM studies reveal the presence of even smaller particles on a nanometer length scale. To eliminate influences of surface irregularities from the crystallization process, acoustic levitation of liquid samples was employed. Such levitated droplets are trapped in a stable position and only surrounded by air. The solvent in an ultrasonically levitated drop evaporates completely, and the resulting crystallization of caffeine was followed in situ by synchrotron X-ray diffraction. In this case, the diffraction pattern is in accordance with pure α-caffeine and does not indicate the formation of the room temperature polymorph β-caffeine. Hence, our investigations open new vistas that may lead to a controlled formation of cocrystals and novel polymorphs of micro- and nanocrystalline materials, which are of relevance for fundamental studies as well as for pharmaceutical and medical applications. KW - Polymorphism KW - Crystallization KW - Acoustic levitation KW - Evaporation of droplets KW - µSpot KW - Micro spot KW - Synchrotron radiation PY - 2008 U6 - https://doi.org/10.1021/la800768v SN - 0743-7463 SN - 1520-5827 VL - 24 IS - 15 SP - 7970 EP - 7978 PB - American Chemical Society CY - Washington, DC AN - OPUS4-17818 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Batzdorf, Lisa A1 - Zimathies, Annett A1 - Panne, Ulrich A1 - Emmerling, Franziska T1 - Mechanochemical synthesis of [Zn3(C2O4)3(4,4'-bipy)4] and its reorganization at high temperatures N2 - The metal organic layered structure catena-(bis(µ2-4,4'-bipyridine)-tris(µ2-oxalato)-bis(4,4'-bipyridine)-tri-zinc(ii)) ([Zn3(C2O4)3(4,4'-bipy)4]) was synthesized mechanochemically applying three different routes. The synthesis succeeded by i) simultaneously neat grinding the three starting materials zinc acetate dihydrate, oxalic acid dihydrate and 4,4'bipyridine, ii) grinding two compounds and adding the third afterwards, independent of the sequence. The products were characterized using powder X-ray diffraction, Raman spectroscopy, gas adsorption measurements, and scanning electron microscopy. Temperature-dependent synchrotron XRD measurements revealed that the monoclinic structure of [Zn3(C2O4)3(4,4'-bipy)4] rearranges reversibly to a higher ordered orthorhombic structure [Zn(C2O4)(4,4'-bipy)] at high temperatures. KW - Mechanochemistry KW - Metal organic compounds KW - Synchrotron radiation KW - Reorganization PY - 2014 U6 - https://doi.org/10.1515/zpch-2014-0445 SN - 0942-9352 SN - 2196-7156 SN - 0044-3336 SN - 0044-3328 SN - 0942-9352 N1 - Geburtsname von Batzdorf, Lisa: Tröbs, L. - Birth name of Batzdorf, Lisa: Tröbs, L. VL - 228 IS - 4-5 SP - 575 EP - 585 PB - Oldenbourg CY - München AN - OPUS4-30628 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wolf, S. E. A1 - Müller, L. A1 - Barrea, R. A1 - Kampf, C.J. A1 - Leiterer, Jork A1 - Panne, Ulrich A1 - Hoffmann, T. A1 - Emmerling, Franziska A1 - Tremel, W. T1 - Carbonate-coordinated metal complexes precede the formation of liquid amorphous mineral emulsions of divalent metal carbonates N2 - During the mineralisation of metal carbonates MCO3 (M = Ca, Sr, Ba, Mn, Cd, Pb) liquid-like amorphous intermediates emerge. These intermediates that form via a liquid/liquid phase separation behave like a classical emulsion and are stabilized electrostatically. The occurrence of these intermediates is attributed to the formation of highly hydrated networks whose stability is mainly based on weak interactions and the variability of the metal-containing pre-critical clusters. Their existence and compositional freedom are evidenced by electrospray ionization mass spectrometry (ESI-MS). Liquid intermediates in non-classical crystallisation pathways seem to be more common than assumed. PY - 2011 U6 - https://doi.org/10.1039/c0nr00761g SN - 2040-3364 SN - 2040-3372 IS - 3 SP - 1158 EP - 1165 PB - RSC Publ. CY - Cambridge AN - OPUS4-23355 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schlegel, Moritz-Caspar A1 - Müller, Urs A1 - Panne, Ulrich A1 - Emmerling, Franziska T1 - Deciphering the sulfate attack of cementitious materials by high-resolution micro-x-ray diffraction N2 - The durability of cementitious materials depends, among others, on their resistance against chemical attack during the service life of a building. Here, we present an approach to analyze changes in the phase composition due to chemical attack in the form of sulfate ingress within the microstructure. Micro-X-ray (µX-ray) diffraction using synchrotron radiation in Debye–Scherrer (transmission) geometry allowed a spatial resolution of 10 µm. Phase transformations in the wake of damaging processes were observed in a detailed high-resolution imaging study. In comparison, samples containing supplementary cementitious materials were investigated and used to reconstruct the influence of different degeneration processes in detail. Additionally, reaction fronts within the bulk were localized by micro-X-ray fluorescence analysis. The experimental setup provided the possibility for analyzing the phase assemblage of a given sample without destroying the microstructure. The specimens for phase analysis are thick sections of the primary material and can be used for further microscopic analysis of the microstructure and microchemistry, e.g., scanning electron microscopy–energy-dispersive X-ray spectroscopy (SEM–EDX) or Raman spectroscopy. PY - 2011 U6 - https://doi.org/10.1021/ac200181g SN - 0003-2700 SN - 1520-6882 VL - 83 IS - 10 SP - 3744 EP - 3749 PB - American Chemical Society CY - Washington, DC AN - OPUS4-23669 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -