TY - CONF A1 - Richter, S. T1 - The Belousov-Zhabotinsky reaction as an engine for the directed transportation of macroscopic particles on surfaces T2 - 24th Conference of the European Colloid and Interface Society CY - Prague, Czech Republic DA - 2010-09-05 PY - 2010 AN - OPUS4-21383 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Almagro, J.-F. A1 - Busch, P. A1 - Gohil, D. D. A1 - Heikinheimo, E. A1 - Karduck, P. A1 - Richter, S. A1 - Sloof, W. G. A1 - Thiot, J.-F. A1 - Wirth, Thomas T1 - Electron-Probe MICROanalysis of LighT Elements - Measurement Methods and Certified Reference Materials (MICROLITE) PY - 2002 IS - 65 SP - 1 EP - 156 PB - National Physical Laboratory CY - Teddington, Middlesex AN - OPUS4-1911 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Richter, S. A1 - Traulsen, C. H.-H. A1 - Heinrich, Thomas A1 - Poppenberg, J. A1 - Leppich, C. A1 - Holzweber, Markus A1 - Unger, Wolfgang A1 - Schalley, C.A. T1 - Sequence-programmable multicomponent multilayers of nanometer-sized tetralactam macrocycles on gold surfaces N2 - Multicomponent multilayers have been deposited on gold surfaces by metal-ion-mediated layer-by-layer self-assembly of differently functionalized tetralactam macrocycles. The layer stack can be programmed with respect to the sequences of metal ions and macrocycles by the deposition sequence. KW - Organic layer KW - XPS KW - SIMS KW - NEXAFS PY - 2013 DO - https://doi.org/10.1021/jp405492v SN - 1932-7447 SN - 1089-5639 VL - 117 IS - 37 SP - 18980 EP - 18985 PB - Soc. CY - Washington, DC AN - OPUS4-32576 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Heinrich, Thomas A1 - Traulsen, Christoph Hans-Henning A1 - Holzweber, Markus A1 - Richter, S. A1 - Kunz, V. A1 - Kastner, S.K. A1 - Krabbenborg, S.O. A1 - Huskens, J. A1 - Unger, Wolfgang A1 - Schalley, C.A. T1 - Coupled molecular switching processes in ordered mono- and multilayers of stimulus-responsive rotaxanes on gold surfaces N2 - Interfaces provide the structural basis for function as, for example, encountered in nature in the membrane-embedded photosystem or in technology in solar cells. Synthetic functional multilayers of molecules cooperating in a coupled manner can be fabricated on surfaces through layer-by-layer self-assembly. Ordered arrays of stimulus-responsive rotaxanes undergoing well-controlled axle shuttling are excellent candidates for coupled mechanical motion. Such stimulus-responsive surfaces may help integrate synthetic molecular machines in larger systems exhibiting even macroscopic effects or generating mechanical work from chemical energy through cooperative action. The present work demonstrates the successful deposition of ordered mono- and multilayers of chemically switchable rotaxanes on gold surfaces. Rotaxane mono- and multilayers are shown to reversibly switch in a coupled manner between two ordered states as revealed by linear dichroism effects in angle-resolved NEXAFS spectra. Such a concerted switching process is observed only when the surfaces are well packed, while less densely packed surfaces lacking lateral order do not exhibit such effects. KW - Molecular machine KW - Rotaxane KW - LBL growth KW - XPS KW - NEXAFS KW - SIMS PY - 2015 DO - https://doi.org/10.1021/ja512654d SN - 0002-7863 SN - 1520-5126 VL - 137 IS - 13 SP - 4382 EP - 4390 PB - American Chemical Society CY - Washington, DC, USA AN - OPUS4-33077 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kelly, U. A1 - Richter, S. A1 - Schladitz, K. A1 - Scheuerlein, C. T1 - Nb3Sn wire shape and cross sectional area inhomogeneity in Rutherford cables N2 - During Rutherford cable production the wires are plastically deformed and their initially round shape is distorted. Using X-ray absorption tomography we have determined the 3D shape of an unreacted Nb3Sn 11 T dipole Rutherford cable, and of a reacted and impregnated Nb3Sn cable double stack. State-of-theart image processing was applied to correct for tomographic artefacts caused by the large cable aspect ratio, for the segmentation of the individual wires and subelement bundles inside the wires, and for the calculation of the wire cross sectional area and shape variations. The 11 T dipole cable cross section oscillates by 2% with a frequency of 1.24 mm (1/80 of the transposition pitch length of the 40 wire cable). A comparatively stronger cross sectional area variation is observed in the individual wires at the thin edge of the keystoned cable where the wire aspect ratio is largest. T2 - 13th European Conference on Applied Superconductivity, EUCAS 2017 CY - Geneva, Switzerland DA - 17.09.2017 KW - X-ray computer tomography KW - Image processing KW - Superconducting KW - CERN KW - µCT PY - 2017 AN - OPUS4-43493 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Poppenberg, J. A1 - Richter, S. A1 - Traulsen, Ch. H.-H. A1 - Darlatt, Erik A1 - Baytekin, B. A1 - Heinrich, Thomas A1 - Deutinger, P. M. A1 - Huth, K. A1 - Unger, Wolfgang A1 - Schalley, Ch. T1 - Programmable multilayers of nanometer-sized macrocycles on solid support and stimuli-controlled on-surface pseudorotaxane formation N2 - Mechanically interlocked molecules (MIMs) such as rotaxanes and catenanes are capable of mechanical motion on the nanoscale and are therefore promising prototypes for molecular machines in recent nanotechnology. However, most of the existing examples are isotropically distributed in solution, which prohibits concerted movement and with it the generation of macroscopic effects. Thus, arranging them in ordered arrays is of huge interest in recent research. We report the deposition of quite densely packed multilayers of tetralactam macrocycles on gold surfaces by metal-coordinated layer-by-layer self-assembly. Linear dichroism effects in angle-resolved NEXAFS spectra indicate a preferential orientation of the macrocycles. The sequence of the metal ions can be programmed by the use of different transition metal ions at each deposition step. Additionally, reversible on-surface pseudorotaxane formation was successfully realized by repeated uptake and release of axle molecules inside the macrocycles cavities. KW - NEXAFS KW - XPS KW - Supramolecular Chemistry KW - Multilayers KW - Pyridine KW - UV/Vis KW - Macrocycles KW - Pseudorotaxanes PY - 2013 DO - https://doi.org/10.1039/c3sc50558h VL - 4 IS - 8 SP - 3131 EP - 3139 AN - OPUS4-42668 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kelly, U. A1 - Richter, S. A1 - Redenbach, C. A1 - Schladitz, K. A1 - Scheuerlein, C. A1 - Wolf, F. A1 - Ebermann, P. A1 - Lackner, F. A1 - Schoerling, D. A1 - Meinel, Dietmar T1 - Nb3Sn wire shape and cross sectional area inhomogeneity in Rutherford cables N2 - During Rutherford cable production the wires are plastically deformed and their initially round shape is distorted. Using X-ray absorption tomography we have determined the 3D shape of an unreacted Nb3Sn 11 T dipole Rutherford cable, and of a reacted and impregnated Nb3Sn cable double stack. State-of-theart image processing was applied to correct for tomographic artefacts caused by the large cable aspect ratio, for the segmentation of the individual wires and subelement bundles inside the wires, and for the calculation of the wire cross sectional area and shape variations. The 11 T dipole cable cross section oscillates by 2% with a frequency of 1.24 mm (1/80 of the transposition pitch length of the 40 wire cable). A comparatively stronger cross sectional area variation is observed in the individual wires at the thin edge of the keystoned cable where the wire aspect ratio is largest. KW - X-ray absorption tomography KW - Image processing KW - Accelerator magnet coils KW - Superconducting PY - 2018 DO - https://doi.org/10.1109/TASC.2018.2791637 SN - 1051-8223 SN - 1558-2515 VL - 28 IS - 4 SP - Article 4800705, 1 EP - 6 PB - IEEE Journals & Magazines AN - OPUS4-44556 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Meyer, S. A1 - Richter, S. A1 - Balski, Matthias A1 - Hagendorf, C. ED - Thirsk, M. T1 - Trace element analysis in crystalline silicon PY - 2013 SN - 978-0-9565331-3-5 SP - 34 EP - 38 PB - Photovoltaics International CY - London, UK AN - OPUS4-29823 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Meyer, S. A1 - Timmel, S. A1 - Richter, S. A1 - Werner, M. A1 - Gläser, M. A1 - Swatek, S. A1 - Braun, Ulrike A1 - Hagendorf, C. T1 - Silver nanoparticles cause snail trails in photovoltaic modules N2 - After some months of operation, a number of PV modules develop a discolouration defect called 'snail trails', or 'snail traces', which appear as irregular dark stripes across the cells. Whereas these traces were soon identified as discoloured silver contacts along the cell edges or at micro cracks, the chemical and mechanistic reasons for this phenomenon have not yet been resolved in detail. In this work we show that silver nanoparticles accumulating within the encapsulation foil cause the brownish discolouration, and that certain additives of encapsulation and back sheet foils trigger the formation of these nanoparticles. KW - Snail trails KW - Cell cracks KW - Encapsulation foil KW - Ag contact finger KW - Nanoparticles PY - 2014 DO - https://doi.org/10.1016/j.solmat.2013.11.013 SN - 0927-0248 VL - 121 SP - 171 EP - 175 PB - Elsevier B.V. CY - Amsterdam [u.a.] AN - OPUS4-30059 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Darlatt, Erik A1 - Nefedov, A. A1 - Traulsen, C.H.-H. A1 - Poppenberg, J. A1 - Richter, S. A1 - Dietrich, Paul A1 - Lippitz, Andreas A1 - Illgen, René A1 - Kühn, Julius A1 - Schalley, C.A. A1 - Wöll, Ch. A1 - Unger, Wolfgang T1 - Interperetation of experimental N K NEXAFS of azide, 1,2,3-triazole and terpyridyl groups by DFT spectrum simulations N2 - Experimental N K-edge NEXAFS data of surface immobilized azide, 1,2,3-triazole and terpyridyl groups are interpreted with the help of DFT spectrum simulations. Assignments of π* resonances in experimental N K-edge NEXAFS spectra to nitrogen atoms within these functional groups have been made. The azide was immobilized on gold as the head group of a thiol SAM, 1,2,3-triazole was formed on this SAM by click reaction and terpyridyl groups were introduced as substituents of the acetylene used for the click reaction. For azide-terminated molecules, DFT spectrum simulations are found to be useful to find measurement conditions delivering experimental N K-edge NEXAFS data with negligible X-ray damage. The 1,2,3-triazole group is found to be rather stable under X-ray irradiation. KW - N K-edge NEXAFS KW - XANES KW - Surface click chemistry KW - Density functional theory KW - Azide KW - 1,2,3-Triazole PY - 2012 DO - https://doi.org/10.1016/j.elspec.2012.09.008 SN - 0368-2048 SN - 1873-2526 VL - 185 IS - 12 SP - 621 EP - 624 PB - Elsevier CY - Amsterdam AN - OPUS4-27774 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Traulsen, C. H.-H. A1 - Kunz, V. A1 - Heinrich, Thomas A1 - Richter, S. A1 - Holzweber, Markus A1 - Schulz, A. A1 - von Krbek, L. K. S. A1 - Scheuschner, U. T. J. A1 - Poppenberg, J. A1 - Unger, Wolfgang A1 - Schalley, C. A. T1 - Synthesis and coordinative layer-by-layer deposition of pyridine-functionalized gold nanoparticles and tetralactam macrocycles on silicon substrates N2 - Coordination chemistry was applied to deposit pyridine-functionalized gold nanoparticles on silicon substrates. The particles were synthesized through the Brust/Schiffrin route with a subsequent ligand exchange reaction yielding well-defined particles of two different sizes. Multilayer deposition was carried out on a pyridine-terminated SAM, anchored on a hydroxyl-terminated silicon surface. Analogously, Hunter/Vögtle-type tetralactam macrocycle multilayers were deposited as well as mixed layers containing both either in an alternating sequence or as a macrocycle multilayer with a terminating nanoparticle layer. These composite layers were examined with respect to their ability to bind squaraine axles in the macrocycle cavities. The amount of guest bound is higher for the composite layer with alternating macrocycles and nanoparticles. KW - Layer-by-layer deposition KW - Functionalized Au nanoparticles KW - SEM KW - TEM KW - DLS KW - XPS KW - NEXAFS KW - ToF-SIMS KW - IR KW - UV-vis PY - 2013 DO - https://doi.org/10.1021/la403222x SN - 0743-7463 SN - 1520-5827 VL - 29 IS - 46 SP - 14284 EP - 14292 PB - American Chemical Society CY - Washington, DC AN - OPUS4-29699 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Heinrich, Thomas A1 - Traulsen, Christoph Hans-Henning A1 - Darlatt, Erik A1 - Richter, S. A1 - Poppenberg, J. A1 - Traulsen, N.L. A1 - Linder, I. A1 - Lippitz, Andreas A1 - Dietrich, Paul A1 - Dib, B. A1 - Unger, Wolfgang A1 - Schalley, C.A. T1 - The versatility of 'Click' reactions at surfaces: Molecular recognition at interfaces N2 - In order to investigate molecular recognition on surfaces, an azide-functionalized monolayer was deposited on gold. The monolayer was characterized by X-ray photoelectron spectroscopy (XPS) and angle-resolved near-edge X-ray absorption fine structure (NEXAFS) experiments and the decomposition of the azide upon irradiation with X-ray beams was investigated. Subsequently, various alkyne-functionalized host and guest molecules were attached to the azide by 1,3-dipolar cycloaddition. These modified surfaces and their host–guest chemistry were analysed by XPS and angle-resolved NEXAFS. The reversibility of guest binding was shown for one example as a proof of principle. KW - 'Click' reaction KW - Azide-terminated surfaces KW - SAMs KW - Host guest molecules KW - Molecular recognition at interfaces PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-306463 DO - https://doi.org/10.1039/C4RA01730G SN - 2046-2069 VL - 4 IS - 34 SP - 17694 EP - 17702 PB - RSC Publishing CY - London AN - OPUS4-30646 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Holzweber, Markus A1 - Heinrich, T. A1 - Kunz, V. A1 - Richter, S. A1 - Traulsen, C.H.-H. A1 - Schalley, C.A. A1 - Unger, Wolfgang T1 - Principal component analysis (PCA)-assisted time-of-flight secondary-ion mass spectrometry (ToF-SIMS): a versatile method for the investigation of self-assembled monolayers and multilayers as precursors for the bottom-up approach of nanoscaled devices N2 - The production of high-quality self-assembled monolayers (SAMs) followed by layer-by-layer (LbL) self-assembly of macrocycles is essential for nanotechnology applications based on functional surface films. To help interpret the large amount of data generated by a standard ToF-SIMS measurement, principal component analysis (PCA) was used. For two examples, the advantages of a combination of ToF-SIMS and PCA for quality control and for the optimization of layer-by-layer self-assembly are shown. The first example investigates how different cleaning methods influence the quality of SAM template formation. The second example focuses on the LbL self-assembly of macrocycles and the corresponding stepwise surface modification. KW - ToF-SIMS KW - Principal component analysis KW - Self assembled monolayer KW - Layer by layer PY - 2014 DO - https://doi.org/10.1021/ac500059a SN - 0003-2700 SN - 1520-6882 VL - 86 IS - 12 SP - 5740 EP - 5748 PB - American Chemical Society CY - Washington, DC AN - OPUS4-30963 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Richter, S. A1 - Poppenberg, J. A1 - Traulsen, C.H.-H. A1 - Darlatt, Erik A1 - Sokolowski, A. A1 - Sattler, D. A1 - Unger, Wolfgang A1 - Schalley, C.A. T1 - Deposition of ordered layers of tetralactam macrocycles and ether rotaxanes on pyridine-terminated self-assembled monolayers on gold N2 - The deposition of tetralactam macrocycles and the corresponding benzyl ether rotaxanes on gold substrates is investigated for the first time exploiting metallo-supramolecular chemistry. Two pyridine-terminated self-assembled monolayers (SAMs) are developed that are used as well-ordered template layers. The two SAMs differ with respect to the rigidity of the terminal pyridines as shown by angle-resolved near-edge X-ray absorption fine structure (NEXAFS) spectroscopy. The template layers are then used for the metal-mediated self-assembly of macrocylces and rotaxanes on solid supports. The SAM with the more rigid terminal pyridine shows a higher coverage with the macrocycles and is therefore preferable. Angle-resolved NEXAFS spectroscopy also shows the deposited supramolecules to be oriented preferentially upright. This order is only achieved for the macrocycles through the deposition on the more rigid SAM template, whereas rotaxanes form oriented layers on both SAMs. Time-of-flight secondary-ion mass spectrometry analysis was used to determine the deposition time required for the self-assembly process. PY - 2012 DO - https://doi.org/10.1021/ja306212m SN - 0002-7863 SN - 1520-5126 VL - 134 IS - 39 SP - 16289 EP - 16297 PB - American Chemical Society CY - Washington, DC AN - OPUS4-26740 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Meyer, S. A1 - Richter, S. A1 - Balski, Matthias A1 - Hagendorf, C. T1 - Trace element analysis in crystalline silicon PY - 2011 SN - 1757-1197 VL - 14th Edition IS - 4th Quarter, November SP - 34 EP - 39 PB - Semiconductor Media CY - London AN - OPUS4-25284 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Poppenberg, J. A1 - Richter, S. A1 - Darlatt, Erik A1 - Traulsen, C.H.-H. A1 - Min, Hyegeun A1 - Unger, Wolfgang A1 - Schalley, C.A. T1 - Successive coordination of palladium(II)-ions and terpyridine-ligands to a pyridyl-terminated self-assembled monolayer on gold N2 - The deposition of palladium on a novel, reversibly protonatable, pyridyl-terminated self-assembled monolayer on gold substrates has been studied by X-ray photoelectron spectroscopy (XPS), near-edge X-ray absorption fine structure spectroscopy (NEXAFS spectroscopy) and time of flight-secondary ion mass spectrometry (ToF-SIMS). For this purpose, 12-(pyridin-4-yl)dodecane-1-thiol, consisting of a surface-active head group, an unfunctionalized hydrocarbon backbone and a terminal pyridyl group, has been synthesized and deposited on gold surfaces. Coordination of Pd(II) ions to the pyridyl group was examined. Furthermore, a reversible protonation/deprotonation cycle has been applied, and the relation between protonation and the amount of complexed palladium was studied. Investigation of the SAM by angle-resolved NEXAFS spectroscopy revealed the aliphatic backbone to be preferentially upright oriented with the aromatic head group being not preferentially oriented. The palladium layer was further coordinated with a CF3-labeled terpyridine ligand in order to prove the accessibility of the Pd(II) ions to further complexation and the platform useful for deposition of further layers toward a multi-layered system. KW - Supramolecular surface chemistry KW - Pyridine terminated monolayer KW - NEXAFS spectroscopy KW - ToF-SIMS KW - Pyridine-metal coordination PY - 2012 DO - https://doi.org/10.1016/j.susc.2011.10.020 SN - 0039-6028 VL - 606 IS - 3-4 SP - 367 EP - 377 PB - Elsevier CY - Amsterdam AN - OPUS4-25282 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Traulsen, C.H.-H. A1 - Darlatt, Erik A1 - Richter, S. A1 - Poppenberg, J. A1 - Hoof, S. A1 - Unger, Wolfgang A1 - Schalley, C.A. T1 - Intermixed terpyridine-functionalized monolayers on gold: nonlinear relationship between terpyridyl density and metal ion coordination properties N2 - Aiming at the functionalization of surfaces with terpyridine anchors for the coordinative deposition of additional layers, mixed self-assembled monolayers (SAMs) were prepared from binary solutions of 12-(2,2':6',2''-terpyridine-4'-yl)dodecane-1-thiol (TDT) and 1-decanethiol (DT). The SAMs and the order of the constituting molecules were analyzed by X-ray photoelectron spectroscopy (XPS), near-edge X-ray absorption fine structure spectroscopy (NEXAFS), and time-of-flight-secondary ion mass spectrometry (ToF-SIMS). The composition of the (TDT/DT)-SAMs and with it the surface density of terpyridyl groups correlates linearly with the relative concentrations of the two compounds in the solution used for depositing them. In marked contrast, the amount of terpyridine-coordinated PdII ions significantly deviates from this trend with an optimum at a 1:3 ratio of TDT/DT. This indicates a major fraction of the terpyridines in TDT-rich SAMs not to be accessible for PdII ion coordination. In agreement, NEXAFS spectroscopy reveals the alkyl backbones in TDT-rich SAMs not to be ordered, while they are preferentially upright oriented in the optimal 1:3-(TDT/DT)-SAMs. We interpret this in terms of terpyridine backfolding in TDT-rich SAMs, while they are located in accessible positions on top of the SAM in the 1:3-(TDT/DT)-SAM. While the alkyl backbones in the 1:3-(TDT/DT)-SAM are ordered, NEXAFS spectroscopy shows the terpyridyl groups not to have a preferential orientation in this SAM and thus retain enough flexibility to adjust to molecules that are deposited on top of the mixed SAM. In conclusion, the novel SAM does not undergo phase separation and consists predominantly of intermixed phases with adjustable surface density of quite flexible terpyridine anchor groups. The terpyridine–PdII anchors are not only available for a future deposition of the next layer, but the metal ions also represent a sensitive probe for the accessibility of the terpyridyl groups. PY - 2012 DO - https://doi.org/10.1021/la301644r SN - 0743-7463 SN - 1520-5827 VL - 28 IS - 29 SP - 10755 EP - 70763 PB - American Chemical Society CY - Washington, DC AN - OPUS4-26430 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Darlatt, Erik A1 - Traulsen, C.H.-H. A1 - Poppenberg, J. A1 - Richter, S. A1 - Kühn, Julius A1 - Schalley, C.A. A1 - Unger, Wolfgang T1 - Evidence of click and coordination reactions on a self-assembled monolayer by synchrotron radiation based XPS and NEXAFS N2 - An ethynylterpyridine was 'clicked' to an azide-terminated self-assembled monolayer on gold and characterized by synchrotron radiation based surface analysis as NEXAFS and XPS. The detection of azide and terpyridine signatures confirmed a partial click reaction at room temperature. The absence of the azides after reaction at 50 °C indicates an almost complete conversion. For the latter case successful Pd(II) coordination has been proven. The Au–S interface of the SAMs has been characterized by S 1s and S 2p XPS. KW - Synchrotron radiation XPS KW - NEXAFS spectroscopy KW - Surface click chemistry KW - Self-assembled monolayer KW - HAXPES KW - XANES PY - 2012 DO - https://doi.org/10.1016/j.elspec.2012.02.004 SN - 0368-2048 SN - 1873-2526 VL - 185 IS - 3-4 SP - 85 EP - 89 PB - Elsevier CY - Amsterdam AN - OPUS4-25596 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Poppenberg, J. A1 - Richter, S. A1 - Traulsen, C.H.-H. A1 - Darlatt, Erik A1 - Baytekin, B. A1 - Heinrich, T. A1 - Deutinger, P.M. A1 - Huth, K. A1 - Unger, Wolfgang A1 - Schalley, C.A. T1 - Programmable multilayers of nanometer-sized macrocycles on solid support and stimuli-controlled on-surface pseudorotaxane formation N2 - Mechanically interlocked molecules (MIMs) such as rotaxanes and catenanes are capable of mechanical motion on the nanoscale and are therefore promising prototypes for molecular machines in recent nanotechnology. However, most of the existing examples are isotropically distributed in solution, which prohibits concerted movement and with it the generation of macroscopic effects. Thus, arranging them in ordered arrays is of huge interest in recent research. We report the deposition of quite densely packed multilayers of tetralactam macrocycles on gold surfaces by metal-coordinated layer-by-layer self-assembly. Linear dichroism effects in angle-resolved NEXAFS spectra indicate a preferential orientation of the macrocycles. The sequence of the metal ions can be programmed by the use of different transition metal ions at each deposition step. Additionally, reversible on-surface pseudorotaxane formation was successfully realized by repeated uptake and release of axle molecules inside the macrocycles cavities. KW - ISO KW - Standard KW - Surface analysis KW - Imaging PY - 2013 DO - https://doi.org/10.1039/c3sc50558h SN - 2041-6520 SN - 2041-6539 VL - 4 SP - 3131 EP - 3139 PB - RSC CY - Cambridge AN - OPUS4-29049 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Richter, S. T1 - Metal Coordinated Layer-by-Layer Self-Assembly of Macrocycles and Rotaxanes on Gold Surfaces T2 - Supramolecules & Assemblies, Chemistry Properties and Organization at Multiple Scales CY - Lucca, Italy DA - 2011-06-19 PY - 2011 AN - OPUS4-23970 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Richter, S. A1 - Horstmann, J. A1 - Altmann, Korinna A1 - Braun, U. A1 - Hagendorf, C. T1 - A reference methodology for microplastic particle size distribution analysis: Sampling, filtration, and detection by optical microscopy and image processing N2 - Microplastic (MP) contamination in natural water circulation is a concern for environmental issues and human health. Various types of polymer materials have been identified and were detected in MP analytic test procedures. Beyond MP polymer type, particle size and form play a major role in water analysis due to possible negative toxicologic effects on flora and fauna. However, the correct quantitative measurement of MP size distribution over several orders of magnitude is strongly influenced by sample preparation, filtration materials and processes, and microanalytical techniques, as well as data acquisition and analysis. In this paper, a reference methodology is presented aiming at an improved quantitative analysis of MP particles. An MP analysis workflow is demonstrated including all steps from reference materials to sample preparation, filtration handling, and MP particle size distribution analysis. Background-corrected particle size distributions (1–1000 µm) have been determined for defined polyethylene (PE) and polyethylene terephthalate (PET) reference samples. Microscopically measured particle numbers and errors have been cross-checked with the total initial mass. In particular, defined reference MP samples (PE, PET) are initially characterized and applied to filtration experiments. Optical microscopy imaging on full-area Si filters with subsequent image analysis algorithms is used for statistical particle size distribution analysis. To quantify the effects of handling and filtration, several blind tests with distilled water are carried out to determine the particle background for data evaluation. Particle size distributions of PE and PET reference samples are qualitatively and quantitatively reproduced with respect to symmetry, and maximum and cut-off diameter of the distribution. It is shown that especially MP particles with a radius of >50 µm can be detected and retrieved with high reliability. For particle sizes <50 µm, a significant interference with background contamination is observed. Data from blank samples allows a correction of background contaminations. Furthermore, for enhanced sampling statistics, the recovery of the initial amount of MP will be qualitatively shown. The results are intended as an initial benchmark for MP analytics quality. This quality is based on statistical MP particle distributions and covers the complete analytic workflow starting from sample preparation to filtration and detection. Microscopic particle analysis provides an important supplement for the evaluation of established spectroscopic methods such as Fourier-transform infrared spectroscopy or Raman spectroscopy. KW - Drinking water KW - Filtration KW - Microplastics detection KW - Quality control KW - Statistical particle distribution PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-567625 DO - https://doi.org/10.1002/appl.202200055 SN - 2702-4288 SP - 1 EP - 10 PB - Wiley-VCH CY - Weinheim AN - OPUS4-56762 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Altmann, Korinna A1 - Abusafia, A A1 - Bannick, C-G A1 - Braun, U A1 - Crasselt, Claudia A1 - Dittmar, S A1 - Fuchs, M A1 - Gehde, M A1 - Hagendorf, C A1 - Heller, C A1 - Herper, D A1 - Heymann, S A1 - Kerndorff, A A1 - Knefel, M A1 - Jekel, M A1 - Lelonek, M A1 - Lunkenbein, T A1 - Obermaier, N A1 - Manhart, M A1 - Meurer, Maren A1 - Miclea, P-T A1 - Paul, A A1 - Richter, S A1 - Ricking, M A1 - Rohner, C A1 - Ruhl, A A1 - Sakai, Y A1 - Saravia Arzabe, C A1 - Scheid, C A1 - Schmitt, M A1 - Schnarr, M A1 - Schwertfirm, F A1 - Steinmetz, H A1 - Wander, Lukas A1 - Wiesner, Yosri A1 - Zechmeister, L T1 - RUSEKU - Repräsentative Untersuchungsstrategien für ein integratives Systemverständnis von spezifischen Einträgen von Kunststoffen in die Umwelt : Abschlussbericht N2 - Im Verbundprojekt RUSEKU wurde die Probenahme von Wasserproben entscheidend weiterentwickelt. Wichtig ist hierbei zu gewährleisten, dass genügend Merkmalsträger in jeder Probe untersucht werden. Es muss daher eine für den Probenahmeort repräsentative Beprobung hinsichtlich des Wasservolumens in Abhängigkeit der Partikelanzahl gewährleistet sein. Das Hauptaugenmerk lag im vorliegenden Projekt auf einer praxisnahen Beprobungsstrategie. Es wurden verschiedene Konzepte ausprobiert. • Grundsätzlich hat sich gezeigt, dass eine Stichprobe eine Momentaufnahme des MP-Massengehaltes zeigt. Es wird eine hohe Statistik, also eine Vielzahl an Messungen am gleichen Probenahmeort, benötigt, um eine valide Aussage über den MP-Gehalt zu machen. • Es zeigt sich, dass eine integrale Probenahme über mehrere Wochen mit dem SK routinemäßig möglich ist. Die erfassten MP-Massen sind reproduzierbar und robust. • Die DFZ ist für Stichproben geeignet. Partikel < 50 µm werden eventuell unterschätzt • Die fraktionierte Filtration kann für Stich- und Mischproben direkt im Feld genutzt werden. Fraktionen von 10 und 5 µm werden später im Labor Vakuum filtriert. Es erfolgt eine Fraktionierung der Probe mit Siebmaschenweiten von 1000, 500, 100, 50, 10 und 5 µm. • Die fraktionierte Filtration kann auch anschließend an die Beprobung mit dem SK zur Anwendung kommen. Wird die mit dem SK gewonnene Wasserprobe fraktioniert filtriert, kann neben einem MP-Gesamtgehalt auch eine Einschätzung über die Partikelgrößen gewonnen werden. • Für Wässer mit geringen Partikelzahlen wurde ein Messfiltertiegel entwickelt. Dieser hat eine Maschenweite von 6 µm. Seine Anwendung kann mögliche Verluste beim Transferieren vom Probenahmetool zum Messgefäß und mögliche Kontaminationen reduzieren. Die Optimierung der Probenahmestrategie wurde durch Modellversuche und Simulationen unterstützt. Modellversuche zum Sinkverhalten und Simulationen von MP in realen Gewässern verdeutlichten das komplexe Verhalten der Partikel. Es konnte gezeigt werden, dass Partikel ab einer bestimmten Größe (und kleiner) bei genügend starker Turbulenz sich in der Wassersäule unabhängig von ihrer Dichte verhalten und so auch MP mit kleiner Dichte (z.B. PE) in der gesamten Wassersäule zu finden sind. Es konnte mit dem TEM die Existenz von NP gezeigt werden. Ein wesentlicher Aspekt des RUSEKU Projektes war die Beprobung realer Kompartimente. Beprobt wurde neben Oberflächengewässern, das urbane Abwassersystem der Stadt Kaiserslautern, Waschmaschinenabwasser und Flaschenwasser. • In Oberflächengewässern wurde hauptsächlich PE gefunden. Je nach Probe und Gewässer konnten auch PP, PS, PET, PA, SBR und Acrylate nachgewiesen werden. • Im urbanen Abwassersystem der Stadt Kaiserslautern konnte an allen Probenahmestandorten MP nachgewiesen werden. Es wurde hauptsächlich PE, neben geringeren Mengen an PP, PS und SBR gefunden. Nach einem Regenereignis war der SBR Anteil deutlich erhöht. • Die Beprobung eines realen Wäschepostens, bestehend aus T-Shirts und Hemden mit PA/CO oder PES/CO Mischgewebe, zeigte einen PA- und PES-Austrag im Waschwasser. Der überwiegende Teil der detektierten Fasern ist aber auf Baumwolle zurückzuführen. Reine gravimetrische Messungen zur Detektion von MP führen zu einer starken Überschätzung. • In Flaschenwasser (PET-Flaschen) konnte MP detektiert werden. PET wurde nur im stillen Mineralwasser, nicht in Mineralwasser mit Kohlensäure gefunden werden. Teilweise wurde auch das MP-Material des Verschlusses im Wasser detektiert. • Für Luftproben konnte ein Aufbau zur größenselektiven Beprobung getestet werden. Neben der Probenahme hat das Projekt auch gezeigt, dass die TED-GC/MS geeignet für die MP-Detektion im Routinebetrieb ist. Die TED-GC/MS konnte weiter optimiert werden. Es wurden MP-Massen bestimmt. Im Projekt wurden erste realitätsnahe Referenzmaterialien für die MP Detektion hergestellt. Die Herstellung von realitätsnahen Polymeren in ausreichender Homogenität und Menge hat sich als große Herausforderung herausgestellt. KW - Mikroplastik KW - Probennahme KW - TED-GC/MS KW - Fraktionierte Filtration KW - Mikroplastikreferenzmaterial PY - 2022 SP - 1 EP - 201 AN - OPUS4-57800 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -