TY - CONF A1 - Goedecke, Caroline A1 - Eisentraut, Paul A1 - Kittner, Maria A1 - Altmann, Korinna A1 - Müller, Axel A1 - Braun, Ulrike T1 - Analysis of microplastics in theory and in practice N2 - Due to the favorable properties of polymers, their production and thus their input into the environment has increased significantly in recent decades. Currently, FTIR or Raman spectroscopy are mainly applied for the analysis of microplastic particles (MP) in environmental samples. However, these methods have great difficulties in determining metrologically traceable MP values, especially with regard to the limiting values, as preferred in regulation. Therefore, we developed a systematic and fast thermoanalytical method called TED-GC-MS (thermal extraction desorption gas chromatography mass spectrometry), which determines mass contents. Now the current goal is the determination of its process parameters. This poster illustrates the theoretical requirements for MP analysis (left side) and contrast them with the current state of research (right side).Unexpected practical problems are presented and the relatively new method is discussed concerning the quality requirements of well-established methods such as LC-or GC-MS. T2 - Eurachem Workshop - Uncertainty from sampling and analysis for accredited laboratories CY - Berlin, Germany DA - 19.11.2019 KW - Microplastics KW - TED-GC-MS KW - Reference materials PY - 2019 AN - OPUS4-49665 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Meyer, A. A1 - Weidner, Steffen A1 - Kricheldorf, H. T1 - Stereocomplexation of cyclic polylactides with each other and with linear poly(L-lactide)s N2 - Two kinds of cyclic poly(D- and L-lactide)s were synthesized, namely CI labeled samples mainly consisting of even-numbered cycles with low dispersity and CII, CIII or CIV-labeled ones consisting of equal amounts of even and odd-numbered cycles with high dispersity and igher molecular weights (Mw up to 300 000). Furthermore, linear poly L-lactide)s were prepared by initiation with ethanol and in both series the molecular weight was varied. The formation of stereocomplexes from cyclic poly(D-lactide)s and all kinds of poly L-lactide)s was performed in dichloromethane/toluene mixtures. The stereocomplexes crystallized from the reaction mixture were characterized in the virgin state and after annealing at 205 °C. Stereocomplexes free of stereohomopolymers with crystallinities up to 80% were obtained from all experiments in yields ranging from 60 to 80%. Despite the high annealing temperature (maintained for 1 h), little transesterification was observed and the crystallinity slightly increased. KW - Polylactide KW - MALDI-TOF MS KW - Stereocomplex KW - Cyclic PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-496693 DO - https://doi.org/10.1039/c9py01236b VL - 10 SP - 6191 EP - 6199 PB - Royal Society for Chemistry AN - OPUS4-49669 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rühle, Bastian A1 - Bresch, Harald A1 - Resch-Genger, Ute A1 - Hodoroaba, Vasile-Dan A1 - Radnick, Jörg T1 - Perspektive der BAM auf neuartige Materialien N2 - Neuartige Materialien, die bekannte (Werk-)Stoffe mit neuen Funktionalitäten ausstatten, spielen eine zunehmend wichtige Rolle im Bereich der Materialforschung und -prüfung. Das Spektrum neuartiger Materialien reicht von der gezielten Oberflächenfunktionalisierung und -strukturierung makroskopischer Materialien, dünnen Beschichtungen bis hin zu mikro- und nanoskaligen Kompositmaterialien und funktionalen Materialien an der Schnittstelle zur Biologie, Biotechnologie, nachhaltige Energiespeicherung und Sensorik. Dabei bieten neuartige Materialien die Chance, Werkstoffe und Produkte mit erweiterter oder verbesserter Funktionalität zu erhalten und Sicherheit bereits im Designprozess zu berücksichtigen. Durch dieses breite Anwendungsspektrum und die Herausforderungen, die solche Materialien für die Sicherheit in Chemie und Technik mit sich bringen, sind diese in allen Themenfeldern der BAM repräsentiert (Material, Analytical Sciences, Energie, Infrastruktur und Umwelt). Die Aufgaben der BAM erstrecken sich dabei von der Herstellung von Referenzmaterialien für Industrie, Forschung und Regulation, über die Erstellung von standardisierten Referenzverfahren für nachhaltige Messungen im Umwelt- und Lebenswissenschaftsbereich bis hin zur Bereitstellung von belastbaren und zitierbaren Referenzdaten. Durch die genaue Charakterisierung neuartiger Materialien können potentiell problematische Substanzen identifiziert und deren Risiken besser abgeschätzt werden. In diesem Beitrag werden einige aktuelle Beispiele aus diesen Bereichen vorgestellt. T2 - NanoDialog der Bundesregierung - Chancen und Risiken von Neuartigen Materialien CY - Berlin, Germany DA - 22.05.2019 KW - Advanced Materials KW - Nanomaterialien KW - Neuartige Materialien PY - 2019 AN - OPUS4-49594 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Henning, L. M. A1 - Simon, U. A1 - Gurlo, A. A1 - Smales, Glen Jacob A1 - Bekheet, M. F. T1 - Grafting and stabilization of ordered mesoporous silica COK-12 with graphene oxide for enhanced removal of methylene blue N2 - Large-pore ordered mesoporous silica (OMS) COK-12, analogous to the well-known SBA-15, but synthesized in a more environmentally friendly way and exhibiting a shorter plate-like structure, was grafted with different amounts of graphene oxide (GO) for the first time in an inexpensive and rapid process, that was successfully upscaled. Samples were examined with nitrogen sorption analysis, SAXS, Raman spectroscopy, XPS, and zeta potential analysis. Adsorption experiments with the cationic dye methylene blue (MB) were conducted on the grafted materials and on pure COK-12, taking into account the influence of initial dye concentration (30–600 mg L-1), adsorbent dosage (0.2–14 g L-1), contact time (0.3–300 min), solution pH (4 10), and influence of salts and temperature (0–1 M NaCl, 80 C) to simulate industrial dye effluent. The adsorption process was found to be represented best by the Langmuir isotherm model, i.e., adsorption is a monolayer process. The calculated maximum Adsorption capacities were found to be 20.2 and 197.5 mg g-1 at dosages of 5 and 0.5 g L-1 for pure COK-12 and COK-12 grafted with 50 wt% GO, respectively, at pH 5.65 and MB concentration of 100 mg L-1. Adsorption kinetics were found to follow the pseudo-second order model, i.e., chemisorption is the rate controlling step. The adsorption performances could be well preserved at simulated dye effluent. Desorption was found to be most effective with hydrochloric acid. The COK-12 grafted with GO presented in this work shows superior adsorption properties in comparison to other grafted OMS materials. In addition, grafting with GO remarkably improved the stability of COK-12 in aqueous solution. KW - COK-12 KW - Mesoporous Silica KW - Graphene Oxide KW - Large-pore PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-497788 UR - https://pubs.rsc.org/en/content/articlehtml/2019/ra/c9ra05541j DO - https://doi.org/10.1039/c9ra05541j VL - 9 IS - 62 SP - 36271 EP - 36284 PB - Royal Society of Chemistry AN - OPUS4-49778 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wurzler, Nina A1 - Wagner, Ralph A1 - Schutter, Jan David A1 - Das, Chayanika A1 - Dimper, Matthias A1 - An, Biwen Annie A1 - Koerdt, Andrea A1 - Lützenkirchen-Hecht, Dirk A1 - Özcan Sandikcioglu, Özlem T1 - Effect of cultivation conditions on the electrochemical activity of metal reducing bacteria (mrb) on stainless steel surfaces N2 - Investigation of the electrochemical activity of two cultures grown with and without abundance of Fe(III) and their different ability to reduce and therefore dissolve iron oxides in steel and model iron thin films. T2 - Eurocorr2019 CY - Sevilla, Spain DA - 09.09.2019 KW - X-ray spectroscopic techniques KW - Microbiologically influenced corrosion KW - MIC KW - XANES KW - Metal reducing bacteria KW - In situ PY - 2019 AN - OPUS4-49692 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, H. A1 - Rademann, K. T1 - Insights into mechanochemical Knoevenagel condensations N2 - Mechanochemistry paves the way to simple, fast, and green syntheses. Despite considerable effort, there is a lack in understanding of the underlying mechanisms. In situ investigations help to understand these mechanisms, which occur during a mechanochemical reaction. Here we present a universal strategy for simultaneous real-time in situ analysis, combining X-ray diffraction, Raman spectroscopy, and thermography. The potential of of our approach is shown for diffrent model reactions. T2 - Adlershofer Forschungsforum 2019 CY - Berlin, Germany DA - 11.11.2019 KW - Mechanochemistry KW - In situ KW - Knoevenagel condensation PY - 2019 AN - OPUS4-49694 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stroh, Julia A1 - Emmerling, Franziska T1 - In situ full phase analysis of the early cement hydration N2 - Fresh cement paste is a suspension consisting of a hydraulic binder (cement), water, and numerous minor components – admixtures. Addition of admixtures aims at specific modification of properties of the fresh cement paste or hardened cementitious building material. Specific admixtures, so-called superplasticizers (SP), are used to improve the flowability of the fresh cement paste with reduced water content. The latter is the starting material for the high-strength concrete. Thus, SPs are essential for the ambitious construction projects. However, uncontrollable retardation of the setting time in presence of SPs is occasionally observed. Obviously, SPs influence early products of the cement hydration leading to changes in the microstructure development. The hardening is thus delayed, and the quality of the resulting building material suffers. The mechanisms of the admixture action during the hydration process are still intensively investigated [1-7]. A detailed understanding of the admixture effects during the early hydration stage is the key to control and individual adjustment of the cement-based construction materials. We use the unique combination of the wall-free sample holder and the time-resolved X-ray scattering analysis to achieve the full information about the hydrate phases formed under the influence of admixtures. We use ultrasonic levitator to start the cement hydration in levitated cement pellets [8, 9]. The sample levitation allows collection of the unimpaired information about cement hydrate phases. The most beneficial is the avoiding of the contributions of the sample holder material to the data signal. We induce the cement hydration by adding water to unhydrated Portland cement during the data acquisition. The full phase composition of the hydrating cementitious system can be gathered in situ using wide angle X-ray scattering (WAXS). During the hydration of cement both crystalline and amorphous hydrate phases are formed. WAXS data contain the information about crystalline phases behind the Bragg reflections, whereas the amorphous hydrates influence the appearance of the background. Application of the data analysis specific for crystalline or amorphous phases is needed. The data quantification by the Rietveld method allows to conclude about the changes of the phase amounts due to the presence of admixture. The calculation of the pair distribution functions allows analysis of the amorphous hydrates. Based on this information, the SP effects and the extent of their involvement into the ongoing reactions can be concluded. A detailed understanding of the complex cement hydration process is envisioned. T2 - Anakon 2019 CY - Münster, Germany DA - 25.03.2019 KW - Cement KW - Admixtures KW - Pair Distribution Functions KW - X-ray diffraction KW - Total scattering analysis PY - 2019 AN - OPUS4-47664 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 - In situ investigations of mechanochemical reactions N2 - Mechanochemistry paves the way to simple, fast, and green syntheses. Despite considerable effort, there remains a lack in understanding of the underlying mechanisms. In situ investigations help to understand these mechanisms, which occur during a mechanochemical reaction. Here we present a universal strategy for simultaneous real-time in situ analysis, combining X-ray diffraction, Raman spectroscopy, and thermography. The potential of our approach is shown for different model reactions. T2 - ANAKON 2019 CY - Münster, Germany DA - 25.03.2019 KW - In situ KW - Mechanochemistry KW - Milling PY - 2019 AN - OPUS4-47701 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fischer, Daniel A1 - Beck, Uwe A1 - Schneider, S. A1 - Duwe, M T1 - Visualisierung von mikro- und nanoskalierten Oberflächenstrukturen mittels abbildender Ellipsometry N2 - In den letzten Jahren hat die Einbindung der abbildenden Ellipsometrie in die Gruppe der optischen Verfahren zur Oberflächencharakterisierung ein enormes Potential bei der Analyse von topologischen Strukturänderungen gezeigt. Der dabei abgebildete Kon-trast wurde typischerweise auf Änderungen im Brechungsindex, Absorptionseffekte oder Schichtdickenänderungen zurückgeführt. In späteren Studien wurde festgestellt, dass auch andere Faktoren, wie etwa die Krümmung der Oberfläche oder Kanten von Struktu-ren einen signifikanten Einfluss auf die Messung der ellipsometrischen Paramater haben. Um diese Effekte aus der ellipsometrischen Messung extrahieren zu können, wird auf die Analyse der Müller-Matrix zurückgegriffen. In dem hier vorliegenden Beitrag wird gezeigt, wie die Müller-Matrix-Imaging Ellipsomet-rie (MM-IE) zur Charakterisierung von Oberflächenstrukturen verwendet werden kann. Dazu werden mikro- und nanoskaliert gekrümmte Oberflächen zunächst mit verschiede-nen Referenzmethoden, wie Rasterelektronenmikroskopie (SEM), Lichtmikroskopie (OM), Weißlichtinterferenzmikroskopie (WLIM) und Rasterkraftmikroskopie (AFM) vali-diert erfasst. Der anschließende Vergleich mit den Ergebnissen der Müller-Matrix-Ima-ging-Ellipsometrie ermöglicht eine Korrelation der zugrunde liegenden Strukturphäno-mene mit den ellipsometrischen Daten. In diesem Artikel wird das Prinzip an drei industriell relevanten Strukturgruppen demonstriert: Sub-Mikropartikel, Mikropartikel und sub-mikroskalierte Vertiefungen. T2 - 14. ThGOT Thementage Grenz- und Oberflächentechnik CY - Zeulenroda, Germany DA - 12.03.2019 KW - Ellipsometrie KW - Nanoskaliert KW - Mikroskaliert KW - Oberflächengeometrie KW - Brechungsindex KW - Müller-Matrix-Ellipsometrie PY - 2019 AN - OPUS4-47645 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fischer, Daniel A1 - Beck, Uwe T1 - Visualisierung von mikro- und nanoskalierten Oberflächenstrukturen mittels abbildender Ellipsometrie N2 - In den letzten Jahren hat die Einbindung der abbildenden Ellipsometrie in die Gruppe der optischen Verfahren zur Oberflächencharakterisierung ein enormes Potential bei der Analyse von topologischen Strukturänderungen gezeigt. Der dabei abgebildete Kon-trast wurde typischerweise auf Änderungen im Brechungsindex, Absorptionseffekte oder Schichtdickenänderungen zurückgeführt. In späteren Studien wurde festgestellt, dass auch andere Faktoren, wie etwa die Krümmung der Oberfläche oder Kanten von Struktu-ren einen signifikanten Einfluss auf die Messung der ellipsometrischen Paramater haben. Um diese Effekte aus der ellipsometrischen Messung extrahieren zu können, wird auf die Analyse der Müller-Matrix zurückgegriffen. In dem hier vorliegenden Beitrag wird gezeigt, wie die Müller-Matrix-Imaging Ellipsomet-rie (MM-IE) zur Charakterisierung von Oberflächenstrukturen verwendet werden kann. Dazu werden mikro- und nanoskaliert gekrümmte Oberflächen zunächst mit verschiede-nen Referenzmethoden, wie Rasterelektronenmikroskopie (SEM), Lichtmikroskopie (OM), Weißlichtinterferenzmikroskopie (WLIM) und Rasterkraftmikroskopie (AFM) vali-diert erfasst. Der anschließende Vergleich mit den Ergebnissen der Müller-Matrix-Ima-ging-Ellipsometrie ermöglicht eine Korrelation der zugrunde liegenden Strukturphäno-mene mit den ellipsometrischen Daten. In diesem Artikel wird das Prinzip an drei industriell relevanten Strukturgruppen demonstriert: Sub-Mikropartikel, Mikropartikel und sub-mikroskalierte Vertiefungen. T2 - 14. ThGOT Thementage Grenz- und Oberflächentechnik und 6. Kolloquium Dünne Schichten in der Optik CY - Zeulenroda, Germany DA - 12.03.2019 KW - Ellipsometrie KW - Nanoskaliert KW - Mikroskaliert KW - Oberflächengeometrie KW - Brechungsindex KW - Müller-Matrix-Ellipsometrie PY - 2019 SN - 978-3-00-062102-4 SP - 1 EP - 5 AN - OPUS4-47646 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lange, Thorid A1 - Hidde, Gundula A1 - Beck, Uwe A1 - Naumann, F. A1 - Kärkkänen, I. A1 - Gargouri, H. T1 - Nanoskalige Haftvermittler zur Erhöhung der Haft- bzw. Klebfestigkeit unter Verwendung von ALD-Hybridprozessen N2 - Ziel des Projektes HARFE (Haftfestigkeit Reproduzierbarkeit Festigkeit) war es, eine Er-höhung der Haft- bzw. Klebfestigkeit auf Niedrigenergie-Polymeren (PE, PP, PTFE) zu erreichen. SENTECH realisierte dazu plasmachemische Oberflächenaktivierungen mit O2 und die Abscheidung von Aluminiumoxidschichten (Al2O3) mittels Atomic Layer Deposition (ALD), wobei die Ellipsometrie zum in-situ Monitoring der ALD-Prozesse diente. Die BAM charakterisierte die modifizierten Oberflächen bezüglich der Oberflächenenergie (OFE) und bestimmte die Verbund- bzw. Klebfestigkeit mittels der Zentrifugentechnologie T2 - 14. ThGOT Thementage Grenz- und Oberflächentechnik und 6. Kolloquium Dünne Schichten in der Optik CY - Zeulenroda, Germany DA - 12.03.2019 KW - Haftvermittler KW - ALD-Hybridprozesse KW - Klebfestigkeit KW - Atomic Layer Deposition KW - Al2O3-Schichten KW - Oberflächenenergie PY - 2019 AN - OPUS4-47653 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lange, Thorid A1 - Hidde, Gundula A1 - Beck, Uwe A1 - Naumann, F. A1 - Kärkkänen, I. A1 - Gargouri, H. T1 - Nanoskalige Haftvermittler zur Erhöhung der Haft- bzw. Klebfestigkeit unter Verwendung von ALD-Hybridprozessen N2 - Ziel des Projektes HARFE (Haftfestigkeit Reproduzierbarkeit Festigkeit) war es, eine Er-höhung der Haft- bzw. Klebfestigkeit auf Niedrigenergie-Polymeren (PE, PP, PTFE) zu erreichen. SENTECH realisierte dazu plasmachemische Oberflächenaktivierungen mit O2 und die Abscheidung von Aluminiumoxidschichten (Al2O3) mittels Atomic Layer Deposition (ALD), wobei die Ellipsometrie zum in-situ Monitoring der ALD-Prozesse diente. Die BAM charakterisierte die modifizierten Oberflächen bezüglich der Oberflächenenergie (OFE) und bestimmte die Verbund- bzw. Klebfestigkeit mittels der Zentrifugentechnologie T2 - 14. ThGOT Thementage Grenz- und Oberflächentechnik und 6. Kolloquium Dünne Schichten in der Optik CY - Zeulenroda, Germany DA - 12.03.2019 KW - Haftvermittler KW - ALD-Hybridprozesse KW - Klebfestigkeit KW - Atomic Layer Deposition KW - Al2O3-Schichten KW - Oberflächenenergie PY - 2019 SN - 978-3-00-062102-4 SP - 1 EP - 2 CY - Zeulenroda, Germany AN - OPUS4-47656 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gramse, G. A1 - Schönhals, Andreas A1 - Kienberger, F. T1 - Nanoscale dipole dynamics of protein membranes studied by broadband dielectric microscopy N2 - We investigate the nearfield dipole mobility of protein membranes in a wide frequency range from 3 kHz to 10 GHz. The results of our nanoscale dielectric images and spectra of bacteriorhodopsin (bR) reveal Debye relaxations with time constants of τ ∼ 2 ns and τ ∼ 100 ns being characteristic of the Dipole moments of the bR retinal and α-helices, respectively. However, the dipole mobility and therefore the protein biophysical function depend critically on the amount of surface water surrounding the protein, and the characteristic mobility in the secondary structure is only observed for humidity levels <30%. Our results have been achieved by adding the frequency as a second fundamental dimension to quantitative dielectric microscopy. The key elements for the success of this advanced technique are the employed heterodyne detection scheme, the broadband electrical signal source, a high frequency optimized cabling, development of calibration procedures and precise finite element modelling. Our study demonstrates the exciting possibilities of broadband dielectric microscopy for the investigation of dynamic processes in cell bioelectricity at the individual molecular level. Furthermore, the technique may shed light on local dynamic processes in related materials science applications like semiconductor Research or nano-electronics. KW - Broadband dielectric microscopy PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-475230 DO - https://doi.org/10.1039/c8nr05880f SN - 2040-3372 VL - 11 IS - 10 SP - 4303 EP - 4309 PB - RSC AN - OPUS4-47523 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kleinbub, Sherin A1 - An, Biwen Annie A1 - Heidrich, Gabriele A1 - Özcan Sandikcioglu, Özlem A1 - Schenderlein, Matthias A1 - Dommisch, H. A1 - Wagner, D. A1 - Koerdt, Andrea T1 - Investigation of the corrosion potential by oral microorganisms related to periodontitis and peri-implantitis N2 - Since the early 19th century microorganisms were studied on their capabilities of causing microbiologically influenced corrosion (MIC) of metals. The most studied ones are sulfate-reducing bacteria (SRB), but others can corrode metals as well, e.g. acid-producing bacteria or methanogenic archaea (MA). However, these studies were mostly focused on metals related to the petroleum industry but metals for other industries, e.g. dentistry, are also susceptible to corrosion. The inert Titanium (Ti) is often used as an implant material, but it is a base metal. The formation of a passivating oxide layer allows Ti to be corrosion resistant at normal conditions. Nonetheless, scanning electron microscope images on dental implants from patients with acute peri-implantitis showed clear signs of corrosion. Currently, the corrosion mechanism of dental implants is unknown, but many indications suggest that oral microorganisms, including MA (Methanobrevibacter oralis) and SRB (Desulfomicrobium orale), could be involved. To determine if MA or SRB can corrode Ti (pure Ti or Ti-6Al-4V alloy), corrosion rate, methane and sulfide concentrations were analyzed. Electrical potential measurements using in-house developed electrochemical cells indicated a potential change on Ti in the presence of a corrosive MA strain compared to an abiotic control. Microbial composition comparison will be analyzed using samples from dental pockets of 150 infected patients by considering the quality of the implant and 50 healthy people by means of amplicon sequencing. Enrichments and isolation of pure cultures from the dentals samples are also examined for their corrosion behavior. Overall, this is the first study investigating the susceptibility of dental implant material to corrosion using human related MA. T2 - Annual Conference of the Association for General and Applied Microbiology CY - Mainz, Germany DA - 17.03.2019 KW - Methanogens KW - Microbiologically Influrenced Corrosion (MIC) KW - Biofilm PY - 2019 AN - OPUS4-47600 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kricheldorf, Hans A1 - Weidner, Steffen A1 - Scheliga, Felix T1 - Ring-Expansion Polymerization (REP) of L-lactide with cyclic Tin(II) Bisphenoxides N2 - Five new cyclic catalysts were prepared by a new synthetic method from tin(II)-2-ethyhexanoate and silylated catechols, silylated 2,2´dihydroxybiphenyl or silylated 1,1´-bisnaphthol. These catalysts were compared with regard to their usefulness as catalysts for the ring expansion polymerization (REP) of L-lactide in bulk at 160 °C, and with two different tin(IV) derivatives of 1,1´binaphthol. Best results were obtained using seven-membered cyclic tin(II)bisphenoxides, which yielded colorless cyclic poly(l-lactide)s free of racemization with weight average molecular weights (Mw) up to 305 000 g mol-1. Furthermore, these catalysts were active even at a lactide/catalyst ratio of 20 000/1. Our new results were superior to those obtained from all other previously published catalysts yielding cyclic poly(L-lactide). The seven-membered cycles also proved to be more active than tin(II) 2-ethylhexanoate with and without the addition of alcohol. KW - Lactide KW - Cyclization KW - Ring-expansion polymerization KW - Tin(II)octanoate KW - MALDI-TOF MS PY - 2019 DO - https://doi.org/10.1016/j.eurpolymj.2019.04.024 SN - 0014-3057 SN - 1873-1945 VL - 116 SP - 256 EP - 264 PB - Elsevier Ltd. AN - OPUS4-47794 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nikitin, D. A1 - Madkour, Sherif A1 - Pleskunov, P A1 - Tafiichuk, R A1 - Shelemin, A A1 - Hanus, J A1 - Gordeev, I A1 - Sysolyatina, E A1 - Ermolaeva, S A1 - Titov, V A1 - Schönhals, Andreas A1 - Choukourov, A T1 - Cu nanoparticles constrain segmental dynamics of crosslinked polyethers: a trade -off between non-fouling and antibacterial properties N2 - Copper has a strong bactericidal effect against multi-drug resistant pathogens and polyethers are known for their resistance to biofilm formation. Herein, we combined Cu nanoparticles (NPs) and a polyether Plasma polymer in the form of nanocomposite thin films and studied whether both effects can be coupled. Cu NPs were produced by magnetron sputtering via the aggregation in a cool buffer gas whereasolyether layers were synthesized by Plasma-Assisted Vapor Phase Deposition with poly(ethylene oxide) (PEO) used as a precursor. In situ specific heat spectroscopy and XPS analysis revealed the formation of a modified polymer layer around the NPs which propagates on the scale of a few nanometers from the Cu NP/polymer interface and then transforms into a bulk polymer phase. The chemical composition of the modified layer is found to be ether-deficient due to the catalytic influence of copper whereas the bulk polymer Phase exhibits the chemical composition close to the original PEO. Two cooperative glass transition phenomena are revealed that belong to the modified polymer layer and the bulk phase. The former is characterized by constrained mobility of polymer segments which manifests itself via a 30 K increase of dynamic glass transition temperature. Furthermore, the modified layer is characterized by the heterogeneous structure which results in higher fragility of this layer as compared to the bulk phase. The Cu NPs/polyether thin films exhibit reduced Protein adsorption; however, the constrained segmental dynamics leads to the Deterioration of the non-fouling properties for ultra-thin polyether coatings. The films are found to have a bactericidal effect against multi-drug resistant Gram-positive Methicillin-Resistant Staphylococcus aureus and Gram-negative Pseudomonas aeruginosa. KW - Nanocomposites KW - Specific heat spectroscopy PY - 2019 DO - https://doi.org/10.1039/c8sm02413h VL - 15 IS - 13 SP - 2884 EP - 2896 PB - RSC AN - OPUS4-47765 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Yin, Huajie A1 - Schönhals, Andreas A1 - Böhning, Martin T1 - Molecular Mobility and Charge Transport in Polymers of Intrinsic Microporosity (PIMs) as Revealed by Dielectric Spectroscopy N2 - Polymeric membranes represent a low-cost, energy efficient solution for gas separation. Recently polymers of intrinsic microporosity (PIMs) have emerged as prestigious membrane materials featuring a large concentration of pores smaller than 1 nm, a BET surface area larger than 700 m2/g and high gas permeability and selectivity. Unusual chain structure combining rigid segments with sites of contortion gives rise to the intrinsic microporosity. However, this novel class of glassy polymers are prone to pronounced physical aging. The initial microporous structures approach a denser state via local small scale fluctuataions, leading to a dramatic reduction in the gas permeabilities. For the first time, dielectric relaxation spectroscopy with state-of-the-art high-resolution analyzers was employed to investigate three representative PIMs with a systematic change in chain rigidity: PIM-EA-TB 〉 PIM-1 〉 PIM-MDPH-TB. The molecular mobility, the charge transport and their response upon heating (aging) in the polymers were measured in a broad temperature range through isothermal frequency scans during different heating / cooling cycles. Multiple dielectric processes following Arrhenius behavior were observed for the investigated polymers. Local fluctuations, Maxwell-Wagner-Sillars (MWS) polarization and structural relaxation phenomena were discussed and attempted to be correlated with the structural features of PIMs. Moreover, all PIMs showed conductivity in the glassy state. The significant increase in the conductivity with increasing temperature far below the glass transition temperature of PIMs is explained in terms of the loosely packed microporous structure and the formation of local intermolecular agglomerates due to interaction of π-electrons in aromatic moieties of the polymer backbone. T2 - American Chemical Society (ACS) National Meeting & Expo 2019 CY - Orlando, FL, USA DA - 31.03.2019 KW - Dielectric spectroscopy KW - Polymeric membrane KW - Polymers of intrinsic microporosity PY - 2019 AN - OPUS4-47805 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Yin, Huajie A1 - Chua, Y. Z. A1 - Yang, B. A1 - Schick, C. A1 - Böhning, Martin A1 - Schönhals, Andreas T1 - Probing the glass transition temperature of polymers of intrinsic microporosity (PIMs) by fast scanning calorimeter N2 - High performance polymers of intrinsic microporosity (PIMs) have emerged as novel materials with broad applications from gas separation to electronic devices. Sufficiently rigid, even contorted polymer chains show only limited molecular mobility, therefore undergo inefficient packing and give rise to intrinsic microporosity with pore size generally smaller than 1 nm and BET surface areas larger than 700 m2/g. Further performance optimization and long-term stability of devices incorporating PIMs rely on our understanding of structure-processing-property relationships and physical aging, in which glass transition plays a key role. Up to now no glass transition temperature (Tg) of PIMs could be detected with conventional thermal analysis techniques before degradation. Decoupling the time scales responsible for the glass transition and the thermal decomposition is a reliable strategy to overcome this. This was achieved by employing fast scanning calorimetry (FSC) based on a chip sensor, which is capable to heat and cool a small sample (ng-range) with ultrafast rates of several ten thousand K/s. FSC provides definitive evidence of glass transition of a series of PIMs with a special consideration on the chain rigidity. The determined glass transition temperature of these PIMs follows the order of the rigidity of their backbone structures. FSC provides the first clear-cut experimental evidence of the glass transition of PIM-EA-TB with a Tg of 663 K, PIM-1 of 644 K and PIM-DMDPH-TB of 630 K at a heating rate of 1Χ104 K/s. Local fluctuations are featured in glass transition of highly rigid PIMs. As conformational changes are prevented by the backbone rigidity, the glass transition must rather be assigned to local small scale fluctuations. T2 - American Chemical Society (ACS) National Meeting & Expo 2019 CY - Orlando, FL, USA DA - 31.03.2019 KW - Glass transition KW - Polymers of intrinsic microporosity KW - Fast scanning calorimeter PY - 2019 AN - OPUS4-47806 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Yildirim, Arda A1 - Bühlmeyer, A. A1 - Hayashi, S. A1 - Haenle, J. C. A1 - Sentker, K. A1 - Huber, P. A1 - Laschat, S. A1 - Schönhals, Andreas T1 - Molecular Dynamics of Dipole Functionalized Triphenylene-based Discotics N2 - In this study, the molecular dynamics of a series of dipole functionalized triphenylene-based discotics, forming a columnar mesophase, were investigated by broadband dielectric spectroscopy (BDS). In addition to conductivity and localized dynamics, glassy dynamics were also observed. At higher temperatures an α1-processes and at low temperatures an α2 processes were detected having a completely different temperature dependence of its relaxation times. Different molecular assignments of α1- and α2-processes are suggested. The phase behavior of the material was explored under helium purge down to 100 K by differential scanning calorimetry (DSC). Besides the phase transition temperatures and enthalpies, one or two thermal glass transitions were found for all the materials. Moreover, the glassy dynamics were further investigated by Flash DSC, which is a chip-based calorimetry technique allowing for fast heating and cooling rates as high as 10000K/s. T2 - Spring Meeting of German Physical Society CY - Regensburg, Germany DA - 01.04.2019 KW - Liquid Crystals PY - 2019 AN - OPUS4-47827 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mitzkus, Anja A1 - Sahre, Mario A1 - Basedau, Frank A1 - Hofman, Detlef A1 - Beck, Uwe T1 - Fiber Bragg Gratings for In-Situ Stress Monitoring of Electrochemical Deposition N2 - The in-situ monitoring of electrochemical deposition (ECD) processes is still a challenge regarding the measurement of the effective temperature of the substrate and the formation of mechanical stress in the layer under given plating conditions. Monitoring problems can be solved by applying a pre-coated fiber Bragg grating (FBG) to the electrolytic process as the shift of the Bragg wavelength is affected by both the temperature of the electrolyte near the substrate and the stress formation in the growing layer. The experimental FBG set-up and the quantitative determination of temperature- and stress-related strain is described for a nickel-iron electrolyte. KW - Fiber Bragg grating (FBG) KW - Electrochemical deposition (ECD) KW - Optical fibers PY - 2019 DO - https://doi.org/10.1149/2.0111906jes SN - 0013-4651 VL - 166 IS - 6 SP - B312 EP - B315 PB - Electrochemical Society CY - Pennington, NJ AN - OPUS4-47738 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Steinhoff, U. A1 - Hodoroaba, Vasile-Dan T1 - EMPIR Erläuterung der Fördermaßnahme und Beispiele aus der Nanotechnologie N2 - Das EMPIR-Förderprogramm wird kurz erläutert und laufende Projekte aus der Nanotechnologie werden vorgestellt. Der Schwerpunkt liegt auf Standardisierungsprojekten, die gemeinsam mit ISO/TC 229 'Nanotechnologies' und CEN/TC 352 'Nanotechnologies' zu neuen Normen führen sollten. Als Beispiel für laufende Nanotechnologie-Projekte mit Koordination aus Deutschland werden MagNaStand (PTB) und nPSize (BAM) gegeben. T2 - Treffen des Normungsausschusses NA 062-08-17 AA Nanotechnologien CY - KIT, Karlsruhe, Germany DA - 07.03.2019 KW - EMPIR KW - Nanoparticles KW - Reference materials KW - Particle size distribution KW - Traceability KW - Standardisation PY - 2019 AN - OPUS4-47859 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Surface and Microbeam Analytical Methods @BAM N2 - An overview of the activities in the field of surface and microbeam analysis at BAM-6.1 is given with focus on physico-chemical characterization at the nanoscale. Ideas of potential joint activities are presented: structural and chemical analysis of graphene, deposition techniques for nanoparticles, EBSD on steel for a broader range of methods, instruments and types of steel, soft X-ray Analysis of low-Z materials, analysis of mesoporous thin films, etc. T2 - BAM-IFW Workshop CY - Dresden, Germany DA - 28.03.2019 KW - PC characterisation KW - Nanoscale KW - Nanoparticles PY - 2019 AN - OPUS4-47860 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN ED - Bosse, H. ED - Buhr, E. ED - Dziomba, T. ED - Hodoroaba, Vasile-Dan ED - Klein, T. ED - Krumrey, M. T1 - NanoWorkshop 2018: Workshop on Reference Nanomaterials N2 - The Scope of the Workshop was to provide a forum for discussion on progress in development, characterisation and application of reference nanomaterials. Results of recently finsihed national and international research projects have been presented. Moreover, the need for future developments have been addressed. Attendees of teh Workshop were expected to be experts from academia, research institutes, regulatory bodies and industry working or interested in the area of reference nanomaterials. The following structure of Workshop was planned: the main focus of the first day was on reference material needs and development, while teh second day was focussed on reference materials characterisation and standardisation. Over 111 participants frm 13 countries and teh European Joint Research Centre have regsitered for the Workshop with 16 platform presentations and 42 poster contributions grouped in 2 sessions and 10 topical areas. A summary of the observations, analysis and conclusions of the Workshop is made including an overview table of links to information on existing reference nanomaterials. KW - Reference Nanomaterials KW - Nanometrology KW - Standardization KW - Nanoparticle Characterization KW - Comparability of Measurement Results KW - Nanomaterial Properties PY - 2019 SN - 78-3-95606-440-1 DO - https://doi.org/10.7795/110.20190412 SN - 0179-0609 VL - 2018 SP - 1 EP - 315 PB - Physikalisch-Technische Bundesanstalt CY - Braunschweig AN - OPUS4-47861 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hampel, Marco A1 - Schenderlein, Matthias A1 - Schary, Christian A1 - Dimper, Matthias A1 - Özcan Sandikcioglu, Özlem T1 - Efficient detection of localized corrosion processes on stainless steel by means of scanning electrochemical microscopy (SECM) using a multi-electrode approach N2 - High resolution analysis of corrosion processes on stainless steels is a challenging task. The application of local electrochemical techniques such as scanning electrochemical microscopy (SECM) has opened new possibilities for the detection of corrosion products and activity on metallic surfaces. However, due to its stochastic nature, the analysis of pitting corrosion requires being at the right place at the right time. Scanning over large areas at a high resolution not only leads to long scan durations but also leaves many short-lived processes undetected. In this paper we present the combined automated operation of SECM and wire multi-electrodes connected to a multi-electrode analyzer (MMA). The inter-electrode currents between 25 wire electrodes connected via zero resistance ammeters (ZRA) are measured by the MMA at open circuit potential (OCP) and the electrodes reporting anodic currents are detected automatically to be analyzed by means of SECM. The results demonstrate the successful application of this methodology for the detection of unstable and stable pitting processes on 304 stainless steel in a corrosive aqueous environment. KW - Scanning electrochemical microscope (SECM) KW - Localised corrosion KW - Corrosion monitoring PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-478646 DO - https://doi.org/10.1016/j.elecom.2019.02.019 VL - 101 SP - 52 EP - 55 PB - Elsevier B.V. AN - OPUS4-47864 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kuchenbecker, Petra A1 - Hodoroaba, Vasile-Dan T1 - Considerations for nanomaterial identification of powders using volume-specific surface area method N2 - The EC’s recommendation for a definition of nanomaterial (2011/696/EU) should allow the identification of a particulate nanomaterial based on the number-based metric criterion according to which at least 50% of the constituent particles have the smallest dimension between 1 and 100 nm. However, it has been recently demonstrated that the implementation of this definition for regulatory purposes is conditioned by the large deviations between the results obtained by different sizing methods or due to practical reasons such as high costs and time-consuming. For most measurement methods for particle size determination it is necessary to initially disperse the particles in a suitable liquid. However, as the particle size decreases, the adhesion forces increase strongly, making it more difficult to deagglomerate the particles and to assess accurately the result of this process. Therefore, the success of the deagglomeration process substantially determines the measurement uncertainty and hence, the comparability between different methods. Many common methods such as dynamic light scattering (DLS), centrifugal liquid sedimentation (CLS) or ultrasound attenuation spectroscopy (US) can give good comparable results for the size of nanoparticles, if they are properly separated and stabilized (e.g. in reference suspensions). In order to avoid the use of hardly available and expensive methods such as SEM / TEM for all powders, an agglomeration-tolerant screening method is useful. One of the measurement methods well suited to probe the size of particulate powder is the determination of the volume-specific surface area (VSSA) by means of gas adsorption as well as skeletal density. The value of 60 m2/cm3 corresponding to spherical, monodisperse particles with a diameter of 100 nm constitutes the threshold for decisioning if the material is a nano- or non-nanomaterial. The identification of a nanomaterial by VSSA method is accepted by the EU recommendation. However, the application of the VSSA method was associated also with some limitations. The threshold of 60 m2/cm3 is dependent on the particle shape, so that it changes considerably with the number of nano-dimensions, but also with the degree of sphericity of the particles. For particles containing micro-pores or having a microporous coating, false positive results are induced. Furthermore, broad particle size distributions made necessary to additionally correct the threshold. Based on examples of commercially available ceramic powders, the applicability of the VSSA approach was tested in relation with SEM and TEM measurements. The introduction of a correction term for deviations from sphericity and further additions improved the applicability of VSSA as a screening method. T2 - Partec CY - Nuremberg, Germany DA - 09.04.2019 KW - VSSA KW - Nanoparticles PY - 2019 AN - OPUS4-47874 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tumanov, I. A1 - Tumanov, E. A1 - Michalchuk, Adam T1 - Ball size or ball mass – what matters in organic mechanochemical synthesis? N2 - Ball mass is an important parameter that is known to have an influence on the outcome of a mechanochemical reaction induced by ball-milling. A standard way of modifying the ball mass is to change the size of the ball made of the same material. In this case, however, a change in mass is accompanied by a simulatneous change in the ball size. It is therefore not possible to disentangle the effects of mass and Surface area in these cases. In the present work we report the results of experiments with specially designed and manufactured balls in which (1) milling ball mass is held constant, but their size differs, and (2) the ball mass is altered, with the diameter of the milling ball being held constant. Using the cocrystallisation of theophylline + nicotinamide as a case study it was found that both diameter and ball mass play crucial roles in determining the rate of a mechanochemical reaction. For comparison, we have also used milling balls with the same size (different mass), and others with the same mass (different size) made of different materials, as would be “traditional”. It was found that, despite having the same size, the lightest milling ball (nylon) was the most efficient in initiating the co-crystallisation, presumably due to the sorption of EtOH. Hence, the results of this manuscript also demonstrate how milling ball material can in fact be the most influential parameter, and potentially counterintuitive to classical mechanics. KW - Mechanochemistry KW - XRD PY - 2019 DO - https://doi.org/0.1039/c8ce02109k VL - 21 SP - 2174 EP - 2179 PB - RSC Royal Society of Chemistry AN - OPUS4-47851 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Szymoniak, Paulina A1 - Madkour, Sherif A1 - Schönhals, Andreas T1 - Molecular dynamics of the asymmetric blend PVME/PS revisited by broadband dielectric and specific heat spectroscopy: Evidence of multiple glassy dynamics N2 - The molecular mobility of the highly asymmetric miscible blend poly(vinyl methyl ether)/polystyrene was investigated by broadband dielectric (frequency range 10^-1 Hz – 10^9 Hz) and specific heat spectroscopy (frequency range 10^1 Hz – 10^4 Hz). The dielectric spectra revealed a complex molecular dynamic behavior, where three different relaxation processes were observed. At temperatures below the glass transition temperature an α´-relaxation was found, with an Arrhenius-like temperature dependence of its relaxation rates. It is assigned to localized fluctuations of the confined PVME segments within a frozen glassy matrix dominated by PS. Above the thermal glass transition temperature two processes with a VFT behavior of their relaxation rates were detected called α1- and α2-relaxation, both originating from PVME dipoles fluctuating in PS-rich environments, however with diverse PS concentrations. The relevant length scales for the processes are assumed to be different, corresponding to the Kuhn segment length for the former relaxation and to the CRR for the latter one. The observed multiple glassy dynamics result from spatial local compositional heterogeneities on a microscopic level. Additionally, SHS investigations were performed for the first time for this system, proving an existence of a fourth relaxation process (α3-relaxation) due to the cooperative fluctuations of both PS and PVME segments. The separation between the thermal α3- and dielectric α2-relaxation increases dramatically with increasing polystyrene concentration, proving that the thermal response is dominated by PS. KW - Polymer blends KW - Dynamic heterogeneity KW - Broadband dielectric spectroscopy KW - Specific heat spectroscopy PY - 2019 DO - https://doi.org/10.1021/acs.macromol.8b02697 SN - 0024-9297 VL - 52 IS - 4 SP - 1620 EP - 1631 PB - ACS Publications AN - OPUS4-47516 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Szymoniak, Paulina T1 - Glass transition and glassy dynamics of thin polymer films and polymer nanocomposites N2 - Polymers at interfaces play a major role in a broad variety of applications ranging from engineering purposes (for instance polymer based nanocomposites) to high tech implications (for instance light emitting diodes). Here the glass transition and glassy dynamics is considered for epoxy-based nanocomposite with Layered Double Hydroxide nanofiller and for thin films of a misicble polymer blend of PVME/PS with thicknesses down to 7 nm. The materials are investigated by spectroscopic techniques (broadband and specific heat spectroscopy), as well as by fast scanning calorimetry and small- and wide-angle X-ray scattering. T2 - Seminarvortrag Columbia University CY - New York, USA DA - 11.03.2019 KW - Nanocomposites KW - Rigid amorphous fraction KW - Thin films KW - Interfaces PY - 2019 AN - OPUS4-47565 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ghasem Zadeh Khorasani, Media A1 - Silbernagl, Dorothee A1 - Elert, Anna Maria T1 - Combination of advanced atomic force microscopy methods to investigate mechanical and chemical interphases in epoxy-boehmite nanocomposites N2 - Formation of interphases between inorganic nanofillers and thermoplastic matrices are usually correlated to short-range interactions which does not exceed more than tens of nanometers away from the surface of the filler. Nevertheless, in nanocomposites with thermosetting matrices, the effect of nanofillers on the properties of the matrix is not limited to the immediate vicinities, but a long-range property alteration of the bulk polymer may be observed. The interaction between nanofillers and the polymer can disturb the curing reaction and alters the chemical, physical and mechanical properties of the polymer network in the matrix phase. In our studies, we aim to investigate short and long-range interphases of a nanocomposite system consisting of a thermosetting matrix (DGEBA) filled with an inorganic nanoparticle (boehmite). For this purpose, a combination of atomic force microscopy (AFM)-based approaches is implemented. Scanning kelvin probe microscopy (SKPM) was used to map the compositional contrast and the interphase with different electrical properties than the bulk. The mechanical properties of the interphase were probed by high resolution intermodulation AFM. (ImAFM). Furthermore, infrared spectroscopy AFM (AFM-IR) is used to investigate the chemical structure of the matrix at different distances from the nanoparticle. SKPM and (AFM-IR) measurements both show a long-range (to 10 µm) effect of boehmite on the chemical structure and surface potential of the bulk epoxy, respectively, whereas ImAFM force measurements reveals a short-range mechanical interphase between the filler and the matrix. The AFM-IR demonstrated the existence of unreacted anhydride hardener at the interphase. This indicates the preferential absorption of anhydride on the surface of boehmite. The consequence of such a selective interaction between the inorganic filler and the epoxy components is disturbance of the epoxy-hardener stoichiometric ratio, the curing mechanism. and the alteration of bulk properties of the matrix. T2 - EUROMAT CY - Stockholm, Sweden DA - 01.09.2019 KW - AFM KW - SKPM KW - AFM-IR KW - ImAFM KW - Boehmite PY - 2019 AN - OPUS4-50693 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ghasem Zadeh Khorasani, Media A1 - Silbernagl, Dorothee A1 - Platz, D. A1 - Sturm, Heinz T1 - Insights into Nano-Scale Physical and Mechanical Properties of Epoxy/Boehmite Nanocomposite Using Different AFM Modes N2 - Understanding the interaction between nanoparticles and the matrix and the properties of interphase is crucial to predict the macroscopic properties of a nanocomposite system. Here, we investigate the interaction between boehmite nanoparticles (BNPs) and epoxy using different atomic force microscopy (AFM) approaches. We demonstrate benefits of using multifrequency intermodulation AFM (ImAFM) to obtain information about conservative, dissipative and van der Waals tip-surface forces and probing local properties of nanoparticles, matrix and the interphase. We utilize scanning kelvin probe microscopy (SKPM) to probe surface potential as a tool to visualize material contrast with a physical parameter, which is independent from the mechanics of the surface. Combining the information from ImAFM stiffness and SKPM surface potential results in a precise characterization of interfacial region, demonstrating that the interphase is softer than epoxy and boehmite nanoparticles. Further, we investigated the effect of boehmite nanoparticles on the bulk properties of epoxy matrix. ImAFM stiffness maps revealed the significant stiffening effect of boehmite nanoparticles on anhydride-cured epoxy matrix. The energy Dissipation of epoxy Matrix locally measured by ImAFM shows a considerable increase compared to that of neat epoxy. These measurements suggest a substantial alteration of epoxy structure induced by the presence of boehmite. KW - Nanomechanics KW - Intermodulation-AFM KW - Interphase KW - Boehmite KW - Epoxy PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-476040 DO - https://doi.org/10.3390/polym11020235 SN - 2073-4360 VL - 11 IS - 2 SP - 235, 1 EP - 19 PB - MDPI AN - OPUS4-47604 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ghasem Zadeh Khorasani, Media A1 - Silbernagl, Dorothee A1 - Szymoniak, Paulina A1 - Hodoroaba, Vasile-Dan A1 - Sturm, Heinz T1 - The effect of boehmite nanoparticles (gamma‐AlOOH) on nanomechanical and thermomechanical properties correlated to crosslinking density of epoxy N2 - We show that complex physical and chemical interactions between boehmite nanoparticles and epoxy drastically affect matrix properties, which in the future will provide tuning of material properties for further optimization in applications from automotive to aerospace. We utilize intermodulation atomic force microscopy (ImAFM) for probing local stiffness of both particles and polymer matrix. Stiff particles are expected to increase total stiffness of nanocomposites and the stiffness of polymer should remain unchanged. However, ImAFM revealed that stiffness of matrix in epoxy/boehmite nanocomposite is significantly higher than unfilled epoxy. The stiffening effect of the boehmite on epoxy also depends on the particle concentration. To understand the mechanism behind property alteration induced by boehmite nanoparticles, network architecture is investigated using dynamic mechanical thermal analysis (DMTA). It was revealed that although with 15 wt% boehmite nanoparticles the modulus at glassy state increases, crosslinking density of epoxy for this composition is drastically low. KW - Crosslinking density KW - Epoxy KW - Intermodulation KW - Atomic force microscopy KW - Nanomechanical properties KW - Boehmite nanoparticles PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-476050 DO - https://doi.org/10.1016/j.polymer.2018.12.054 SN - 0032-3861 SN - 1873-2291 VL - 164 SP - 174 EP - 182 PB - Elsevier AN - OPUS4-47605 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Szymoniak, Paulina A1 - Schönhals, Andreas A1 - Madkour, Sherif T1 - Broadband dielectric spectroscopy on miscible polymer blends in the bulk and in nanometer thick films - Comparison of the different confinement situations N2 - Broadband dielectric spectroscopy in the frequency range from 10-1 to 109 Hz is employed to revisit the segmental dynamics of the miscible blend system poly(vinyl methyl ether)/polystyrene (PVME/PS) in dependence on the composition firstly in the bulk state. Here especially the case of high polystyrene concentrations is considered. It is important to note that only the molecular dynamics of PVME segments as affected by PS is observed because the dipole moment of polystyrene is negligible. Three relaxation processes are found which are due to fluctuations of differently constrained or confined PVME segments. The degree of the confinement of PVME segments due to PS is discussed in dependence on the composition. Further a spatial confinement is considered by investigating thin films of the PVME/PS blend where the film thickness was varied from 100 nm down to 5 nm. Two concentrations of PVME/PS (50/50 wt% and 25/75 wt%) are investigated. To measure nanometer thick films a novel electrode system based on nanostructured electrodes was employed. Nanostructured electrodes can be considered as a cut-edge technology in dielectric spectroscopy. The relaxation spectra of the films showed multiple processes which are discussed in dependence on the film thickness. T2 - Spring Meeting of the American Physical Scociety CY - Boston, Ma, USA DA - 03.03.2019 KW - Polymer blends PY - 2019 AN - OPUS4-47518 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Leng, Jing A1 - Szymoniak, Paulina A1 - Kang, N.-J. A1 - Wang, D-Y A1 - Wurm, A. A1 - Schick, C. A1 - Schönhals, Andreas T1 - Influence of interfaces on the crystallization behavior and the rigid amorphous phase of poly(l-lactide)-based nanocomposites with different layered doubled hydroxides as nanofiller N2 - Based on the three-phase model of semi-crystalline polymers, we determined all phase fractions of the NiAl-LDH/PLLA nanocomposites in dependence on the concentration of the nanofiller. Moreover, the rigid amorphous fraction (RAF) was separated into the RAFcrystal and the RAFfiller unbiasedly. A detailed comparison to the related nanocomposite system MgAl-LDH/PLLA was made considering that Mg and Ni have different atomic weights. As a first result is was found that NiAl-LDH/PLLA displays a higher crystallization rate compared to MgAl-LDH/PLLA, which is related to the different morphologies of the two nanocomposite systems. For both systems RAFcrystal increases with increasing concentration of the nanofiller. This means in the case of the nanocomposite not each crystal produces the same amount of RAF, as often assumed. Also, RAFfiller increases with the concentration for both systems but in a different way. This is discussed considering again the different morphologies of both nanocomposites. KW - Polymer-based nanocomposites KW - Temperature modulated differential scanning calorimetry PY - 2019 DO - https://doi.org/10.1016/j.polymer.2019.121929 VL - 184 SP - 121929 PB - Elesevier Ltd. AN - OPUS4-49557 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Szymoniak, Paulina A1 - Schönhals, Andreas T1 - Rigid amorphous phase in polymer nanocomposites as revealed by dielectric relaxation spectroscopy and fast scanning calorimetry N2 - For inorganic/polymer nanocomposites a so-called Rigid Amorphous Phase (RAF) is formed in the interfacial region by adsorption of polymer segments onto the nanoparticles. The segmental dynamics of RAF is expected to be altered, as compared to the pure matrix, which might percolate into the entire system, affecting the overall nanocomposite properties. A combination of two relaxation spectroscopy techniques (Broadband Dielectric Spectroscopy (BDS) and Specific Heat Spectroscopy (SHS) in a form of Temperature Modulated DSC (TMDSC)) as well as Fast Scanning Calorimetry (FSC) was employed to investigate the structure and molecular mobility of nanocomposites based on Epoxy and Layered Doubled Hydroxides with different nanoparticle content. First, BDS investigations proved the existence of a process, which is present only for nanocomposites, assigned to the dynamics of polymer segments within RAF. Second, the amount of RAF was quantified by analyzing the change of specific heat capacity step of nanocomposites, comparing to the pure material. Thirdly, the glass transition of nanocomposites was studied with FSC, applying high heating rates (500-10 000 K/s). Considering that all techniques probe essentially the same molecular process, an activation plot was constructed, delivering a complete picture of the molecular mobility and structure of the polymer nanocomposites including RAF. T2 - American Physical Society (APS) March Meeting 2019 CY - Boston, MA, USA DA - 04.03.2019 KW - Nanocomposites KW - Rigid amorphous fraction PY - 2019 AN - OPUS4-47564 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Szymoniak, Paulina A1 - Schönhals, Andreas T1 - Rigid Amorphous Phase in Epoxy-based Nanocomposites as Revealed by Dielectric Spectroscopy and Fast Scanning Calorimetry N2 - For inorganic/polymer nanocomposites a so-called Rigid Amorphous Phase (RAF) is formed in the interfacial region by adsorption of polymer segments onto the nanoparticles. The segmental dynamics of RAF is expected to be altered, as compared to the pure matrix, which might percolate to the entire system, affecting the overall nanocomposite properties. A combination of two relaxation spectroscopy techniques (Broadband Dielectric Spectroscopy (BDS) and Temperature Modulated DSC (TMDSC)) as well as Fast Scanning Calorimetry (FSC) was employed to investigate the structure and molecular mobility of nanocomposites based on Epoxy and Layered Doubled Hydroxides with different nanoparticle content. First, BDS investigations proved the existence of a process, which is present only for nanocomposites, assigned to the dynamics of polymer segments within RAF. Second, the amount of RAF was quantified by analyzing the change of specific heat capacity step of nanocomposites, comparing to the pure material. Thirdly, the glass transition of nanocomposites was studied with FSC, applying high heating rates (0.5-10 kK/s). Considering that all techniques probe essentially the same molecular process, an activation plot was constructed, delivering a complete picture of the molecular mobility and structure of the polymer nanocomposites including RAF. T2 - DPG-Frühjahrstagung 2019 CY - Regensburg, Germany DA - 01.04.2019 KW - Rigid amorphous fraction KW - Nanocomposites PY - 2019 AN - OPUS4-47762 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Szymoniak, Paulina A1 - Schönhals, Andreas A1 - Madkour, Sherif T1 - Multiple Glassy Dynamics of an Asymmetric PVME/PS Blend Investigated by Broadband Dielectric and Specific Heat Spectroscopy N2 - Over the past decades research on the molecular dynamics of miscible polymer blends is of topical interest in the literature, to understand the segmental mobility of individual components, as it is affected by blending. In general, miscible polymer blends exhibit a complex dynamic behavior. For an A/B blend the relaxation times of component A and component B are affected by the spatial local compositional heterogeneity, present in binary systems on a microscopic level, regardless of the macroscopic homogeneity. Here, a combination of broadband dielectric and specific heat spectroscopy was employed to study the dynamically asymmetric PVME/PS blend with seven different compositions, focusing on samples with high PS contents. Considering that PS is dielectrically invisible, BDS is a powerful technique to study the response of PVME, as it is affected by PS segments. Here, three separate relaxation processes were found by dielectric investigations, related to confined or constrained PVME segments due to the spatial local compositional heterogeneities, which is in contrary to the previous literature findings [1]. Moreover, the dielectric data was compared with results obtained by specific heat spectroscopy, where a fourth relaxation process was found, due to the cooperative fluctuations of PVME and PS. [1] Colmenero, J., Arbe, A. Soft Matter, 2007, 3, 1474. T2 - DPG-Frühjahrstagung 2019 CY - Regensburg, Germany DA - 01.04.2019 KW - Specific heat spectroscopy KW - Polymer blends KW - Dielectric spectroscopy PY - 2019 AN - OPUS4-47764 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana A1 - Epping, Ruben T1 - View into the Depths of Copolymer Microstructure N2 - For different kinds of polymers it will be shown how it could be realized to obtain information on small, sometimes isomeric topological heterogeneities by coupling UPLC / ESI-TOF-MS and LC /MALDI-TOF-MS. T2 - DSM, Fall Meeting CY - Breda, The Netherlands DA - 07.11.2019 KW - Microstructure KW - LC-MS KW - Copolymer PY - 2019 AN - OPUS4-49587 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana A1 - Epping, Ruben T1 - View into the depths of copolymer microstructure by a special approach of LC-MS data evaluation N2 - It is a well-known story that copolymers beside their molar mass distribution (MMD) can exhibit a functionality type distribution (FTD), a copolymer composition distribution (CCD), a monomer sequence distribution (MSD) and additionally different topologies within one sample. This is and will remain a challenge for analysts. First a very short overview will be given concerning the common liquid separation techniques for polymers (SEC, LAC, LCCC, GELC) coupled to soft ionization mass spectrometric methods like MALDI and ESI-MS with focus on their limitations. For very broadly distributed samples or chemical very similar species the superposition of different separation mechanisms in chromatography is unavoidable or the separation efficiency cannot be optimized. Different ionization probabilities and species of the same nominal mass with completely different structures are just two problems of mass spec of complex polymer mixtures. Subsequently, different examples will be shown how these limitations in some cases could be outsmarted. First example will be the separation of statistical EO-PO copolymers of different chemical compositions by end group functionality and the quantification of end group fractions over the whole CCD. Here an UP-LCCC / ESI-TOF-MS coupling is applied. Further for different kinds of polymers it will be shown how it could be realized to obtain information on small isobaric/isomeric topological heterogeneities by coupling UP-SEC / ESI-TOF-MS. All results are based on the data processing of reconstructed ion chromatograms of single mass traces of complex ESI-MS spectra. T2 - SCM-9 CY - Amsterdam, The Netherlands DA - 29.01.2019 KW - Reconstructed ion chromatograms KW - Copolymer KW - Microstructure KW - LC x ESI-TOF-MS PY - 2019 AN - OPUS4-47836 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schütter, Jan A1 - Pietsch, Franziska A1 - Schreiber, Frank A1 - Koerdt, Andrea A1 - Özcan Sandikcioglu, Özlem T1 - Effect of surface topography and chemistry on the attachment of bacteria on solid surfaces N2 - Microbiologically induced corrosion due to bacterial biofilms causes several problems in industrial systems, technical applications and in medicine. Prior to the formation of a biofilm on a substrate, planktonic cells attach on the surface. Hence, the properties of the surface play a key role in biofilm formation and are of great importance for the development of strategies to prevent bacterial attachment and biofilm formation. This project aims at clarifying to which extent surface micro-/nanostructuring and chemical functionalization affects bacterial attachment and whether a synergistic combination of the two can be used to control bacterial adhesion. To answer these questions, model surfaces with regular patterns of 5-10 micrometers in size have been prepared, which provide distinct zones differing in terms of their chemistry or nano-roughness. This was achieved by micro contact printing of self-assembled monolayers with different functional groups and deposition of patterned ZnO nanorod arrays for studying the effect of surface chemistry and morphology, respectively. Typical contrasts studied were combinations of positively/negatively charged, hydrophobic/hydrophilic or flat/rough. The attachment behavior of bacteria on tailored surfaces were studied in a flow chamber as a function of time. The strain Pseudomonas fluorescens SBW25 was chosen as a model organism. DNA-intercalating dyes such as Syto9 have a high affinity to adsorb on ZnO nanorods. To overcome this limitation a genetic modification was performed by introducing a gene which expresses a green fluorescent protein in P. fluorescens SBW25 enabling the quantitative evaluation of the flow chamber studies by means of fluorescence microscopy. Further analysis of the attachment behavior was performed by means of scanning electron microscopy. The presentation will summarize the results of our systematic study on the role of individual parameters on bacterial attachment and highlight synergistic combinations, showing an inhibition or enhancing effect. As the investigations with model substrates enable a precise control of the surface parameters, this approach can be applied to different microorganisms and material systems to achieve a correlative description of bacterial adhesion on solid surfaces. T2 - Eurocorr2019 CY - Sevilla, Spain DA - 09.09.2019 KW - Microbial KW - Corrosion KW - MIC KW - Nanorods PY - 2019 AN - OPUS4-49730 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Legall, Herbert A1 - Schwanke, Christoph A1 - Bonse, Jörn A1 - Krüger, Jörg T1 - X-ray emission during ultrashort pulse laser processing N2 - The industrial use of ultrashort laser pulses has made considerable progress in recent years. The reasons for this lie in the availability of high average powers at pulse repetition rates in the several 100 kHz range. The advantages of using ultrashort laser pulses in terms of processing precision can thus be fully exploited. However, high laser intensities on the workpiece can also lead to the generation of unwanted X-rays. Even if the emitted X-ray dose per pulse is low, the accumulated X-ray dose can become significant for high-repetition-rate laser systems so that X-ray exposure safety limits must be considered. The X-ray emission during ultrashort pulse laser processing was investigated for a pulse duration of 925 fs at 1030 nm wavelength and 400 kHz repetition rate. Industrially relevant materials such as steel,aluminum and glass were treated. Tungsten served as reference. X-ray spectra were recorded, and X-ray dose measurements were performed for laser treatment in air. For laser intensities > 2 × 10^13 W/cm2, X-ray doses exceeding the regulatory exposure limits for members of the public were found. Suitable X-ray protection strategies are proposed. T2 - SPIE Photonics West CY - San Francisco, USA DA - 02.02.2019 KW - Laser-induced X-ray emission KW - Ultrashort laser material interaction KW - Radiation protection PY - 2019 SN - 978-1-5106-2459-7 DO - https://doi.org/10.1117/12.2516165 SN - 0277-786X SN - 1996-756X VL - 10908 SP - 1090802-1 EP - 1090802-7 PB - SPIE - The international society for optics and photonics CY - Bellingham, WA, USA AN - OPUS4-47510 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bonse, Jörn A1 - Legall, Herbert A1 - Schwanke, Christoph A1 - Krüger, Jörg T1 - Emission von Röntgenstrahlung bei der UKP-Laser-Materialbearbeitung N2 - Der Vortrag stellt Untersuchungen im Rahmen eines BMBF-geförderten Vorhabens zur unerwünschten Emission von Röntgenstahlung bei der Materialbearbeitung mit ultrakurzen Laserpulsen vor. T2 - 7. OptoNet Laserstammtisch “Ultrakurzpulslaser” CY - Jena, Germany DA - 12.03.2019 KW - Laserschutz KW - Materialbearbeitung KW - Röntgenemission KW - Sekundärstrahlung KW - Ultrakurze Laserpulse PY - 2019 AN - OPUS4-47569 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bonse, Jörn A1 - Florian, Camilo A1 - Krüger, Jörg T1 - Quo vadis LIPSS? – Recent developments in theoretical modelling and technical applications N2 - This presentation reviews current and expected developments in the field of laser-induced periodic surface structures (LIPSS, ripples). These surface nanostructures are a universal phenomenon and can be generated on almost any material by irradiation with intense linearly polarized radiation. LIPSS are formed in a “self-ordered” way and are often accompanying laser material processing applications. The structures can be produced in a single-step process and enable surface functionalization through the adaption of optical, mechanical and chemical surface properties. Their spatial periods typically range from several micrometers down to less than 100 nanometers, exhibiting a clear correlation with the polarization direction of the laser radiation used. Various types of LIPSS have been classified, relevant control parameters were identified, and material specific formation mechanisms are analyzed for different types of inorganic solids, i.e., metals, semiconductors, and dielectrics, through time-resolved optical experiments and theoretical simulations. Special attention will be paid to a comparison of the currently available formation theories for LIPSS with a discussion of their respective strengths and weaknesses. Currrently explored applications featuring surface functionalization in the fields of optics, surface wetting, medicine, and tribology will be discussed. T2 - 9th International LIPSS Workshop CY - Ljubljana, Slovenia DA - 26.09.2019 KW - Laser-induced periodic surface structures (LIPSS) KW - Surface functionalization KW - Femtosecond laser ablation KW - Modelling KW - Applications PY - 2019 AN - OPUS4-49708 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Topolniak, Ievgeniia A1 - Hodoroaba, Vasile-Dan A1 - Braun, Ulrike A1 - Pfeifer, Dietmar A1 - Sturm, Heinz T1 - Reinforced UV curable cycloaliphatic epoxy oligosiloxane resin nanocomposite for coating applications N2 - Coating materials are nowadays often required to deliver not only sufficient barrier performance and suited optical appearance but a broad range of other functional properties. The incorporation of inorganic nanoparticles (NPs) is known to improve many key characteristics and provide new functionalities in polymer materials. Presented work aims to prepare and characterize an organic-inorganic coating material designed to bring together advantageous properties of hybrid materials and reinforcement effect delivered from the inorganic NPs embedment. Siloxane-based hybrid resins hold great advantages as coating materials as their properties can be tuned between those of polymers and those of glasses, thus, the compositions with superior thermal and mechanical properties can be achieved. We used Cycloaliphatic Epoxy Oligosiloxane (CEOS) resin as a polymeric matrix where the network formation was achieved by UV induced cationic polymerisation. Boehmite Alumina (BA) nanoparticles were added to CEOS resin as a reinforcing agent and resultant material was processed into films either by bar-coating or by spin-coating depending on further characterization procedure. Two different types of BA NPs, hydrophilic and organophilic, were used in order to assess the impact of particles surface on the resin characteristics. CEOS synthesis by condensation reaction was confirmed using 13C and 29Si NMR. Changes in CEOS photocuring process, resulting from particles incorporation, were monitored by real-time IR spectroscopy. At the same time, the thermal behaviour was evaluated by DSC and TGA methods. Morphology of the coatings was investigated by means of SEM operated in transmission mode. It was observed that BA presence increased the epoxy conversion degree and glass transition temperature. Material formulations providing best film characteristics were determined with regard to the particle type and loading. Compared to the hydrophilic nanoparticles, organophilic BA NPs yield superior overall performance of the foils. T2 - HYMA Conference CY - Sitges, Spain DA - 11.03.2019 KW - Cycloalyphatic epoxy oligosiloxane KW - Nanocomposite KW - Boehmite KW - Photocuring PY - 2019 AN - OPUS4-47641 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gawek, Marcel A1 - Hertwig, Andreas A1 - Schönhals, Andreas T1 - Growth Kinetics and Molecular Mobility of Irreversibly Adsorbed Layers in Thin Polymer Films N2 - In well-annealed thin polymer films, with non-repulsive polymer/substrate interactions, an irreversibly adsorbed layer is formed. These adsorbed layers have shown enormous potential for technological applications. The growth kinetics and molecular dynamics of these buried layers in thin films are still not fully investigated due to the hard accessibility. Here, the irreversibly adsorbed layers of homopolymer thin films are revealed by solvent-leaching experiments. The growth kinetics of these layers is investigated as a function of original film thickness and annealing times. The thickness, topography and quality of the adsorbed layer is determined with Atomic Force Microscopy (AFM) and spectroscopic ellipsometry. Additionally, the molecular mobility of the adsorbed layer is investigated with Broadband Dielectric Spectroscopy (BDS). A recently developed nanostructured capacitor (NSC) is employed to measure the adsorbed layers with a free surface layer depending on annealing and solvent-leaching time. The results are quantitatively compared and discussed with respect to recently published work. T2 - Spring Meeting of German Physical Society CY - Regensburg, Germany DA - 31.03.2019 KW - Adsorbed layer KW - Thin polymeric films PY - 2019 AN - OPUS4-47767 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bonse, Jörn A1 - Legall, Herbert A1 - Schwanke, Christoph A1 - Pentzien, Simone A1 - Krüger, Jörg T1 - X-Ray Emission during Laser Processing with Ultrashort Laser Pulses N2 - Ultrashort laser pulse micromachining features a high precision. By increasing the repetition rate of the applied laser to several 100 kHz, laser processing becomes quick and cost-effective and make this method attractive for industrial applications. Upon exceeding a critical laser intensity, hard X-ray radiation is generated as a side effect. Even if the emitted X-ray dose per pulse is low, the accumulated X-ray dose becomes significant for high-repetition-rate laser systems so that radiation safety must be considered. T2 - 5th UKP-Workshop: Ultrafast Laser Technology CY - Aachen, Germany DA - 10.04.2019 KW - Laser-induced X-ray emission KW - Radiation protection KW - Ultrashort laser material interaction PY - 2019 AN - OPUS4-47788 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Peláez, R.J. A1 - Rebollar, E. A1 - Serna, R. A1 - Acosta-Zepeda, C. A1 - Saavedra, P. A1 - Bonse, Jörn A1 - Haro-Poniatowski, E. T1 - Nanosecond laser-induced interference grating formation on silicon N2 - The formation of gratings on the surface of a silicon wafer by nanosecond laser irradiation through a phase mask using an ArF laser emitting at 193 nm is studied. The phase mask along with some focusing optics is capable to generate via interference a periodic intensity distribution, which can be used for surface patterning. The surface patterning strongly depends on the laser energy density and on the number of pulses, as revealed by atomic force microscopy (AFM). The results show that irradiation even with a single laser pulse produces periodic depth modulations on the surface. The spatial surface modulation is in the micrometer (1.7 µm) range while the depth modulation is in the nanometer regime (1–20 nm). With an increasing number of pulses (1–100), the depth modulation amplitude increases smoothly. Increasing the number of pulses further results in the progressive destruction of the grating, vanishing completely after ~5000 pulses. This evolution is also monitored in situ by measuring the intensity of the first order-diffracted probe beam and the behavior is in accordance with what is observed by AFM. Finally, we qualitatively explain the results invoking thermally induced effects in the melted Si: these physical processes involved are probably thermocapillary and/or Marangoni effects inducing material displacement as the surface melts. KW - Nanosecond laser irradiation KW - Silicon KW - Surface modification KW - Phase mask KW - Grating PY - 2019 UR - https://iopscience.iop.org/article/10.1088/1361-6463/ab0c5f DO - https://doi.org/10.1088/1361-6463/ab0c5f SN - 1361-6463 SN - 0022-3727 VL - 52 IS - 22 SP - 225302, 1 EP - 10 PB - IOP Publishing CY - Bristol, UK AN - OPUS4-47619 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe A1 - Griepentrog, Michael A1 - Hertwig, Andreas A1 - Hielscher, Stefan A1 - Weise, Matthias T1 - Auf dem Weg zu Industrie 4.0: Bestimmung von Messunsicherheitsbudgets in der Oberflächentechnik N2 - Vorgestellt wurde die Bestimmung von Messunsicherheitsbudgets für sehr unterschiedliche physikalische Größen, die in der Oberflächentechnik von hoher Relevanz sind: Stufenhöhe h, Schichtdicke d, Eindringhärte HIT und Haftfestigkeit. Die Unterschiede betreffen die Art der Prüfmethodik (optisch zerstörungsfrei vs. mechanisch invasiv/zer-störend), die laterale Größe des Integrationsgebietes der Messung (lokal:nano bis sub-mikro vs. global: mikro bis makro) und die Art der Bestimmung von Messunsicherheitsbudgets (physikalische Größen: direkt rückführbar; Werkstoffkenngröße: genormt; Systemkenngröße: genormt). Im Rahmen von Industrie 4.0 werden ausgehend der geforderten Spezifikation des beschichteten Produkts (Mittelwert mit Vertrauensbereich oder Mindestwert) durchgehende Toleranzbänder zur Oberflächenmodifizierung/Beschichtung des Substrats, einhergehend mit Prozessfenstern, die diese Toleranzbänder garantieren, erforderlich, die zuverlässig erfasst werden müssen. Die Frage der anzuwendenden Mess- und Prüftechnik und die damit notwendige Betrachtung von Messunsicherheitsbudgets ist für die Digitalisierung von Konditionierungs-, Zustands-, Regel- und Steuergrößen unverzichtbar. Mit Blick auf die Einhaltung von Prozessfenstern und die dafür notwendige Prozessführung wird technologisches Kern-Know-how digitalisiert, das es unbedingt zu schützen gilt. Nur lokale Netze können diese Sicherheit garantieren, in globalen Netzen ist die Datensicherheit bestenfalls maximierbar. T2 - 14. ThGOT Thementage Grenz- und Oberflächentechnik CY - Zeulenroda, Germany DA - 12.03.2019 KW - Oberflächentechnik KW - Messunsicherheit KW - Messtechnik KW - Prüftechnik KW - Haftfestigkeit PY - 2019 AN - OPUS4-47612 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gawek, Marcel A1 - Madkour, Sherif A1 - Hertwig, Andreas A1 - Schönhals, Andreas T1 - Growth Kinetics and Molecular Mobility of Irreversibly Adsorbed Layers in Thin Films of P2VP and PVME N2 - In well-annealed thin polymer films, with non-repulsive polymer/substrate interactions, an irreversibly adsorbed layer is formed. These adsorbed layers have shown enormous potential for technological applications. Due to the hard accessibility of these layers, their growth kinetics and molecular dynamics are still not fully understood. Here, the irreversibly adsorbed layers of Poly(2-vinylpyridine) (P2VP) and Poly(vinyl methyl ether) (PVME) thin films are revealed by solvent-leaching experiments. The growth kinetics of these layers is investigated as a function of original film thickness and annealing times. The thickness, topography and quality of the adsorbed layer is determined with Atomic Force Microscopy (AFM) and spectroscopic ellipsometry. Additionally, the molecular mobility of the adsorbed layer is investigated with Broadband Dielectric Spectroscopy (BDS). A recently developed nanostructured capacitor (NSC) is employed to measure the adsorbed layers with a free surface layer depending on annealing and solvent-leaching time. The results are quantitatively compared and discussed with respect to recently published work. T2 - Spring Meeting of German Physical Society CY - Regensburg, Germany DA - 31.03.2019 KW - Adsorbed layer KW - Thin polymeric films PY - 2019 AN - OPUS4-47766 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Florian, Camilo A1 - Kirner, Sabrina V. A1 - Krüger, Jörg A1 - Bonse, Jörn T1 - Quo vadis LIPSS? – Applications of laser-induced periodic surface structures N2 - Laser-induced periodic surface structures (LIPSS, ripples) are a universal phenomenon that can be observed on almost any material after the irradiation by linearly polarized laser beams, particularly when using ultrashort laser pulses with durations in the femtosecond to picosecond range. During the past years significantly increasing industrial and research activities have been reported in the field of LIPSS, since their generation in a single-step process provides a simple way of nanostructuring and surface functionalization towards the control of optical, mechanical or chemical surface properties. In this contribution the mechanisms of formation and current trends and applications of LIPSS are reviewed, including the colorization of technical surfaces, the control of surface wetting properties, the mimicry of the natural texture of animals, the tailoring of surface colonization by bacterial biofilms, the advancement of leadless medical pacemakers, and the improvement of the tribological performance of nanostructured metal surfaces. T2 - 11. Mittweidaer Lasertagung CY - Mittweida, Germany DA - 13.11.2019 KW - Laser-induced periodic surface structures (LIPSS) KW - Femtosecond laser ablation KW - Surface functionalization KW - Applications PY - 2019 VL - 3/1 SP - 41 EP - 43 PB - Hochschule Mittweida CY - Mittweida AN - OPUS4-49673 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hoevelmann, J. A1 - Stawski, T. M. A1 - Besselink, R. A1 - Freeman, H. M. A1 - Dietmann, K. M. A1 - Mayanna, S. A1 - Pauw, Brian Richard A1 - Benning, L. G. T1 - A template-free and low temperature method for the synthesis of mesoporous magnesium phosphate with uniform pore structure and high surface area N2 - Mesoporous phosphates are a group of nanostructured materials with promising applications, particularly in biomedicine and catalysis. However, their controlled synthesis via conventional template-based routes presents a number of challenges and limitations. Here, we show how to synthesize a mesoporous Magnesium phosphate with a high surface area and a well-defined pore structure through thermal decomposition of a crystalline struvite (MgNH4PO4·6H2O) precursor. In a first step, struvite crystals with various morphologies and sizes, ranging from a few micrometers to several millimeters, had been synthesized from supersaturated aqueous solutions (saturation index (SI) between 0.5 and 4) at ambient pressure and temperature conditions. Afterwards, the crystals were thermally treated at 70–250 °C leading to the release of structurally bound water (H2O) and ammonia (NH3). By combining thermogravimetric analyses (TGA), scanning and transmission electron microscopy (SEM, TEM), N2 sorption analyses and small- and wide-angle X-ray scattering (SAXS/WAXS) we show that this decomposition process results in a pseudomorphic transformation of the original struvite into an amorphous Mg-phosphate. Of particular importance is the fact that the final material is characterized by a very uniform mesoporous structure with 2–5 nm wide pore channels, a large specific surface area of up to 300 m2 g−1 and a total pore volume of up to 0.28 cm3 g−1. Our struvite decomposition method is well controllable and reproducible and can be easily extended to the synthesis of other mesoporous phosphates. In addition, the so produced mesoporous material is a prime candidate for use in biomedical applications considering that Magnesium phosphate is a widely used, non-toxic substance that has already shown excellent biocompatibility and biodegradability. KW - Struvite KW - SAXS KW - Scattering KW - Nanoporous KW - Geology PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-477130 DO - https://doi.org/10.1039/c8nr09205b VL - 11 IS - 14 SP - 6939 EP - 6951 PB - Royal Society of Chemistry AN - OPUS4-47713 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -