TY - CONF A1 - Greiser, Sebastian A1 - Sturm, Patrick A1 - Gluth, Gregor A1 - Hunger, M. A1 - Jäger, Christian T1 - 29Si-27Al NMR to verify and distinguish Qn(mAl) sites in zeolites and geopolymers N2 - One-part-geopolymers, produced by addition of water to a mixture of solid silica and sodium alumi-nate, are a less exhaustively studied approach to form geopolymeric binders. Depending on the silica source, the reaction products show significant amounts of zeolite Na-A besides amorphous compounds. Previously, 29Si MAS NMR has been used to analyze the chemical structure of such one-part geopolymers, having crystalline structures and amorphous phases (Q2, Q3, Q4). In this work, pure zeolites and three different one-part-geopolymers cured for 1 day were investigated by 29Si-27Al TRAPDOR NMR. It was used to identify aluminum phases in overlapping silicon sites. Zeolites Na-X (Si/Al=1.4) and Na-Y (Si/Al=2.7) served as model systems to measure the TRAPDOR effect of the structural units Q4(mAl). Both materials show several Q4(mAl) signals, which are all separated by their chemical shifts. The more aluminum surrounds the silicon tetrahedron the higher are the normalized TRAPDOR difference signals (S0/∆S). The intensity ratios between Q4(mAl) to Q4({m-1}Al) of these signals is fixed but vary slightly between both zeolites. These results are transferred to the complex geopolymer structure. T2 - 57th Experimental nuclear magnetic resonance conference CY - Pittsburgh, PA, USA DA - 10.04.2016 KW - NMR KW - 29Si-27Al TRAPDOR MAS KW - Geopolymer KW - One-part formulation KW - Rice husk ash PY - 2016 AN - OPUS4-35864 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nguyen, Thi Yen A1 - Bernardes, C. A1 - Minas da Piedade, M. E. A1 - Rademann, K. A1 - Emmerling, Franziska T1 - Direct evidence of polyamorphism in paracetamol N2 - While polymorphism is a common phenomenon in the crystallization processes of organic compounds, polyamorphism has gained importance only recently. Using sophisticated sample environments and applying in situ scattering methods and vibrational spectroscopy, the complete crystallization process of organic compounds from solution can be traced and characterized. Diffuse scattering from amorphous intermediates can be investigated by analyzing the atomic pair Distribution function (PDF) to gain further insights into molecular pre-orientation. The crystallization behavior of Paracetamol was studied exemplarily under defined, surface-free conditions. Based on the choice of the solvent, the formation of different polymorphs is promoted. The thermodynamically stable form I and the metastable orthorhombic form II could be isolated in pure form directly from solution. For both polymorphs, the crystallization from solution proceeds via a distinct amorphous precursor phase. PDF analyses of these different amorphous states indicate a specific pre-orientation of the analyte molecules introduced by the solvent. The resulting crystalline polymorph is already imprinted in these proto-crystalline precursors. Direct experimental evidence for the polyamorphism of paracetamol is provided. T2 - Annual CM1402 crystallize COST meeting CY - Coimbra, Portugal DA - 06.04.2016 KW - Paracetamol KW - Crystallization KW - In situ analysis KW - Active pharmaceutical ingredient (API) PY - 2016 AN - OPUS4-35873 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heilmann, Maria A1 - Bienert, Ralf A1 - Prinz, Carsten A1 - Emmerling, Franziska T1 - Synthesis of bimetallic nickel nanoparticles as catalysts for the Sabatier reaction N2 - Nanoparticles (NP) have become important materials for a variety of chemical technologies. The enhanced surface-area-to-volume ratio of NPs, making them excellent for use as catalyst, in analytical assays, and for antimicrobial applications. Nickel NPs have exhibited immense potential as important catalyst for the Sabatier reaction, i.e. converting waste to energy via transformation of CO2 into CH4, and could replace the rare earth elements such as Ru, PT, or Rh. In this work we describe the solvothermal synthesis of monometallic and bimetallic nickel nanoparticles. Monodisperse monometallic Ni NPs were synthesized using Oleylamin as solvent and reducing agent. The nanoparticles were investigated using small angle scattering (SAXS), scanning transmission electron microscopy (STEM) and energy dispersive X-ray spectroscopy (EDX), showing that the NPs are stable while the surface is not entirely covered. However, Ni has a high propensity to undergo oxidation, and becoming deactivated by coke formation. Hence, we further explore the preparation of bimetallic NPs, where a second metal is added to stabilize the Ni. Bimetallic Cu-Ni NPs were synthesized by simultaneous solvothermal reduction. These bimetallic NPs exhibit excellent catalytic properties are promising candidates to be used as catalysts for efficient energy storage. T2 - 31. Tag der Chemie 2019 CY - Berlin, Germany DA - 11.07.2019 KW - Nanoparticles KW - Catalysis KW - Synthesis PY - 2019 AN - OPUS4-50171 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heilmann, Maria A1 - Bienert, Ralf A1 - Prinz, Carsten A1 - Emmerling, Franziska T1 - Synthesis of bimetallic nickel nanoparticles for catalysis N2 - We present the synthesis of monodisperse monometallic Ni nanoparticles (NPs) and bimetallic NiCu respectively NiCo NPs. The NPs were investigated using SAXS, STEM, EDX, and XANES, showing that the NPs are size tunable and stable while the surface is not entirely covered. Nickel NPs have exhibited immense potential as important catalyst for the Sabatier reaction, i.e. converting waste to energy via transformation of CO2 into CH4. T2 - 11th Joint BER II and BESSY II User Meeting CY - Berlin, Germany DA - 04.12.2019 KW - Nanoparticles KW - Catalysis KW - Synthesis PY - 2019 AN - OPUS4-50172 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heilmann, Maria A1 - Bienert, Ralf A1 - Prinz, Carsten A1 - Emmerling, Franziska T1 - Synthesis of bimetallic nickel nanoparticles as catalysts for the Sabatier reaction N2 - Nanoparticles (NPs) have become important materials for a variety of chemical technologies. The enhanced surface-area-to-volume ratio of NPs, making them excellent for use as catalyst, in analytical assays, and for antimicrobial applications. Nickel NPs have exhibited immense potential as important catalyst for the Sabatier reaction, i.e. converting waste to energy via transformation of CO2 into CH4, and could replace the rare earth elements such as Ru, PT, or Rh. In this work we describe the solvothermal synthesis of monometallic and bimetallic nickel nanoparticles. Monodisperse monometallic Ni NPs were synthesized using Oleylamin as solvent and reducing agent. The nanoparticles were investigated using small angle scattering (SAXS), scanning transmission electron microscopy (STEM) and energy dispersive X-ray spectroscopy (EDX), showing that the NPs are stable while the surface is not entirely covered. However, Ni has a high propensity to undergo oxidation, and becoming deactivated by coke formation. Hence, we further explore the preparation of bimetallic NPs, where a second metal is added to stabilize the Ni. Bimetallic Cu-Ni NPs were synthesized by simultaneous solvothermal reduction. These bimetallic NPs exhibit excellent catalytic properties are promising candidates to be used as catalysts for efficient energy storage. T2 - Adlershofer Forschungsforum 2019 CY - Berlin, Germany DA - 11.11.2019 KW - Nanoparticles KW - Catalysis KW - Synthesis PY - 2019 AN - OPUS4-50173 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Haferkamp, Sebastian A1 - Emmerling, Franziska A1 - Akhmetova, Irina A1 - Kulla, Hannes A1 - Rademann, K. T1 - Insights into the mechanochemical Knoevenagel condensation N2 - Mechanochemistry paves the way to simple, fast, and green syntheses, but there is a lack in understanding of the underlying mechanisms. Here, we present a universal strategy for simultaneous real-time in situ analysis, combining X-ray diffraction, Raman spectroscopy, and thermography. T2 - Bessy User Meeting 2019 CY - Berlin, Germany DA - 05.12.2019 KW - Mechanochemistry PY - 2019 AN - OPUS4-50122 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Colini, Claudia A1 - Hahn, Oliver A1 - Rabin, Ira T1 - A black ink by any other name...: Typologies of arabic inks and their detection limits N2 - In this poster we will present some results of a research projects dealing with Arabic recipes of black inks [1-2]. To improve conservation practices of Arabic manuscripts we have assessed the feasibility of the recipes collected from many Arabic sources on bookmaking and reproduced the most common inks. Ink samples were then artificially aged and analysed using an array of analytical techniques, mostly non-invasive, in order to build a database of Arabic inks and their ingredients and also to verify the detection limits of the portable equipment employed. We will show procedures and problems concerning the identification of ink types and ingredients using reflectography (in Vis, IR and UV), X-Ray Fluorescence, Infrared and Raman spectroscopy. The focus will be in particular on squid ink [3] and mixed inks – both in the form of carbon inks with the addition of tannins and of a mixture of carbon and iron gall inks – which are particularly difficult to detect [4]. We will also examine the results of iron gall inks made with iron filings or nails instead of vitriol, the various precursor used to extract gallic acid that are mentioned in the sources as surrogates of gall nuts. [1] A. Schopen, Tinten und Tuschen des arabisch-islamischen Mittelalters, Göttingen: Vandenhoeck & Ruprecht, 2004 [2] S. Fani, Le arti del libro secondo le fonti arabe originali. I ricettari arabi per la fabbricazione degli inchiostri (sec. IX-XIII): loro importanza per una corretta valutazione e conservazione del patrimonio manoscritto, PhD thesis, Napoli: Università L’Orientale, 2013 [3] S. Centeno, J. Shamir Journal of Molecular Structure, 873 (2008), 149-159 [4] C. Colini et. al, Manuscript cultures, 11 (2018) 43-50 T2 - Jahrestagung „Archäometrie und Denkmalpflege 2019“ CY - Vienna, Austria DA - 11.09.2019 KW - Inks KW - Reflectography KW - XRF KW - Raman Spectroscopy KW - ATR PY - 2019 AN - OPUS4-50162 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wilbig, Janka A1 - Borges de Oliveira, F. A1 - Schwentenwein, M. A1 - Günster, Jens T1 - Quality Aspects of Additively Manufactured Medical Implants - Defect Detection in Lattice Parts N2 - Additive Manufacturing technologies are developing fast to enable a rapid and flexible production of parts. Tailoring products to individual needs is a big advantage of this technology, which makes it of special interest for the medical device industry and the direct manufacturing of final products. Due to the fast development, standards to assure reliability of the AM process and quality of the printed products are often lacking. The EU project Metrology for Additively Manufactured Medical Implants (MetAMMI) is aiming to fill this gap by investigating alternative and cost efficient non-destructive measurement methods. T2 - yCAM Forum CY - Mons, Belgium DA - 03.03.2019 KW - Additive Manufacturing KW - Metrology PY - 2019 AN - OPUS4-49141 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mishurova, Tatiana A1 - Artzt, K. A1 - Haubrich, J. A1 - Requena, G. A1 - Bruno, Giovanni T1 - New aspects about the search for the most relevant parameters optimizing SLM materials N2 - Using non-optimum combination of manufacturing parameters in selective laser melting (SLM) may lead to reduction of quality of component: defects generation, distortion of geometry and even cracking. Usually, the optimization of parameters is performed by changing volumetric energy density (Ev) and selecting parameters giving low porosity values. However, not only low porosity but also stable microstructure and low residual stresses will help to achieve advanced mechanical behavior of the component. In present work, we investigated cuboid-shaped Ti-6Al-4V samples produced with different manufacturing parameters. The parameters leading to the same Ev were considered as well as parameters which are not included in Ev. Residual stresses in subsurface region were investigated by synchrotron X-ray diffraction, which allows to penetrate around 100 µm from the surface therefore overcome the problem of high roughness of SLM components without additional sample preparation. Only tensile stresses were found along the building direction, that can play critical role especially during cyclic loading. The pore shape and spatial distribution obtained by computed tomography varied for samples produced with the same Ev. However, by using some process parameters it was possible to decrease residual stresses and obtain uniform α+β Ti microstructure and relatively low porosity. Additionally, it was found that not included in Ev (e.g., base plate position, focus distance) should be considered as additional manufacturing parameters during SLM process. T2 - ESIAM 2019 CY - Trondheim, Norway DA - 09.09.2019 KW - Additive manufacturing KW - Computed tomography KW - Residual stress PY - 2019 AN - OPUS4-49216 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fleck, M. A1 - Tielemann, Christopher A1 - Scheffler, F. A1 - Brauer, D. S. A1 - Müller, Ralf T1 - Surface crystallization of BT0.75S (fresnoite) glass in different atmosphere N2 - Fresnoite glass with excess SiO2 exhibits oriented surface crystallization, in contrast to the stoichiometric glass composition. Recent EBSD studies documented that the crystals in BTS (2BaO-TiO2-xSiO2, x=0-3) can occur in a distinct [101]-orientation perpendicular to the surface and claimed that this orientation is not a result of growth selection. During these previous studies, however, the effect of surface preparation and surrounding atmosphere during the crystallization experiments were not considered. As these parameters may influence crystal orientation, we studied the surface crystallization of a BTS glass (2BaO-TiO2–2.75SiO2) under controlled conditions with the help of light, electron and polarisation microscopy as well as EBSD. Heat treatments for one hour at 840°C of fractured BTS glass surfaces in air resulted in a large number of not-separable surface crystals. This large number of crystals can be caused by dust particles, which act as nucleation agents. As crystal growth velocity could further be influenced by humidity, our experiments are performed in a filtered and dried air atmosphere. The crystal morphology and orientation will be analysed in dependence of the sample preparation and a differing surrounding atmosphere. T2 - 93rd Annual Meeting of the German Society of Glass Technology in Conjunction with the Annual Meeting of French Union for Science and Glass Technology (USTV) CY - Nuremberg, Germany DA - 13.05.2019 KW - BTS KW - Fresnoit KW - Glass ceramic KW - Glass-ceramic KW - Glass PY - 2019 AN - OPUS4-49294 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -