TY - JOUR A1 - Kulla, Hannes A1 - Greiser, Sebastian A1 - Benemann, Sigrid A1 - Rademann, K. A1 - Emmerling, Franziska T1 - In Situ Investigation of a Self-Accelerated Cocrystal Formation by Grinding Pyrazinamide with Oxalic Acid JF - Molecules N2 - A new cocrystal of pyrazinamide with oxalic acid was prepared mechanochemically and characterized by PXRD, Raman spectroscopy, solid-state NMR spectroscopy, DTA-TG, and SEM. Based on powder X-ray diffraction data the structure was solved. The formation pathway of the reaction was studied in situ using combined synchrotron PXRD and Raman spectroscopy. Using oxalic acid dihydrate the initially neat grinding turned into a rapid self-accelerated liquid-assisted grinding process by the release of crystallization water. Under these conditions, the cocrystal was formed directly within two minutes. KW - in situ KW - cocrystal KW - mechanochemistry KW - pyrazinamide KW - hydrate PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-372357 DO - https://doi.org/10.3390/molecules21070917 SN - 1420-3049 VL - 21 IS - 7 SP - Article 917, 1 EP - 9 AN - OPUS4-37235 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Heilmann, Maria A1 - Kulla, Hannes A1 - Prinz, Carsten A1 - Bienert, Ralf A1 - Reinholz, Uwe A1 - de Oliveira Guilherme Buzanich, Ana A1 - Emmerling, Franziska T1 - Advances in Nickel Nanoparticle Synthesis via Oleylamine Route JF - nanomaterials N2 - Nickel nanoparticles are an active research area due to their multiple applications as catalysts in different processes. A variety of preparation techniques have been reported for the synthesis of these nanoparticles, including solvothermal, microwave-assisted, and emulsion techniques. The well-studied solvothermal oleylamine synthesis route comes with the drawback of needing standard air-free techniques and often space-consuming glassware. Here, we present a facile and straightforward synthesis method for size-controlled highly monodisperse nickel nanoparticles avoiding the use of, e.g., Schlenk techniques and space-consuming labware. The nanoparticles produced by this novel synthetic route were investigated using small-angle X-ray scattering, transmission electron microscopy, X-ray diffraction, and X-ray spectroscopy. The nanoparticles were in a size range of 4–16 nm, show high sphericity, no oxidation, and no agglomeration after synthesis. KW - Nanoparticle synthesis KW - Nickel nanoparticles KW - SAXS KW - TEM KW - XAS PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-507531 DO - https://doi.org/10.3390/nano10040713 VL - 10 IS - 4 SP - 713 PB - MDPI AN - OPUS4-50753 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -