TY - CONF A1 - Özcan Sandikcioglu, Özlem T1 - Nanotechnology at BAM N2 - The presentation gives a brief summary of the research activities of BAM in the field of nanotechnology. It was held at INERIS in the frame of a delegation meeting to identify topics for future collaborations. T2 - Kooperationstreffen mit INERIS CY - Verneuil-en-Halatte, France DA - 23.10.2017 KW - Nanotechnology KW - Nano Referenzmaterialien KW - Nanosafety PY - 2017 AN - OPUS4-43408 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Özcan Sandikcioglu, Özlem A1 - Kastanias, Elaine A1 - Wurzler, Nina A1 - Hampel, Marco T1 - Spektroelektrochemische Analyse der Korrosionsprozesse von eisenreduzierenden Mikroorganismen N2 - Der Vortrag ist eine Zusammenfassung der Forschungsaktivitäten im FB 6.2 im Rahmen des Themenfeldprojekts MIC (TF-Material). T2 - DECHEMA/GfKORR-Fachgruppe "Mikrobielle Materialzerstörung und Materialschutz" CY - Berlin, Germany DA - 04.10.2017 KW - Korrosion KW - Mikrobiell induzierte Korrosion (MIC) KW - Lokale Elektrochemie KW - Spektroelektrochemie KW - Oberflächenverstärkte Raman Spektroskopie (SERS) KW - XANES PY - 2017 AN - OPUS4-43462 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zscherpel, Uwe A1 - Ewert, Uwe T1 - Annual report of sub-commission V-A "Radiography based weld inspection" N2 - Annual report on activities of sub-commission V-A of the International Institute of Welding given by its chairman. T2 - Annual Assembly of IIW CY - Shanghai, China DA - 25.06.2017 KW - Radiographic testing KW - International Institute of Welding PY - 2017 AN - OPUS4-41135 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zhang, Zhiyang A1 - Merk, V. A1 - Müller, Anja A1 - Unger, Wolfgang A1 - Kneipp, Janina T1 - Role of metal cations in plasmon-catalyzed oxidation: A case study of p-aminothiophenol dimerization JF - ACS Catalysis N2 - The mechanism of the plasmon-catalyzed reaction of p-aminothiophenol (PATP) to 4,4′-dimercaptoazobenzene (DMAB) on the surface of metal nanoparticles has been discussed using data from surface-enhanced Raman scattering of DMAB. Oxides and hydroxides formed in a plasmon-catalyzed process were proposed to play a central role in the reaction. Here, we report DMAB formation on gold nanoparticles occurring in the presence of the metal cations Ag+, Au3+, Pt4+, and Hg2+. The experiments were carried out under conditions where formation of gold oxide or hydroxide from the nanoparticles can be excluded and at high pH where the formation of the corresponding oxidic species from the metal ions is favored. On the basis of our results, we conclude that, under these conditions, the selective oxidation of PATP to DMAB takes place via formation of a metal oxide from the ionic species in a plasmon-catalyzed process. By evidencing the necessity of the presence of the metal cations, the reported results underpin the importance of metal oxides in the reaction. KW - Metal ions KW - Plasmonic catalysis KW - p-aminothiophenol KW - 4,4'-dimercaptoazobenzene KW - Surface-enhanced Raman scattering PY - 2017 UR - http://pubs.acs.org/doi/abs/10.1021/acscatal.7b02700 DO - https://doi.org/10.1021/acscatal.7b02700 SN - 2155-5435 N1 - Geburtsname von Müller, Anja: Hermanns, A. - Birth name of Müller, Anja: Hermanns, A. VL - 7 IS - 11 SP - 7803 EP - 7809 PB - American Chemical Society CY - Washington AN - OPUS4-43001 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zhang, Rui A1 - Russo, Patrícia A. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Jeon, Taeyeol A1 - Pinna, Nicola T1 - Hybrid organic–inorganic transition-metal phosphonates as precursors for water oxidation electrocatalysts JF - Advanced Functional Materials N2 - Efficient water oxidation catalysts are required for the development of water splitting technologies. Herein, the synthesis of layered hybrid NiFephenylphosphonate compounds from metal acetylacetonate precursors and phenylphosphonic acid in benzyl alcohol, and their Oxygen evolution reaction performance in alkaline medium, are reported. The hybrid particles are formed by inorganic layers of NiO6 and FeO6 distorted octahedra separated by bilayers of the organic group, and template the Formation in situ of NiFe hydroxide nanosheets of sizes between 5 and 25 nm and thicknesses between 3 and 10 nm. X-ray absorption spectroscopy measurements suggest that the hybrid also acts as a template for the local structure of the metal sites in the active catalyst, which remain distorted after the transformation. Optimum electrocatalytic activity is achieved with the hybrid compound with a Fe content of 16%. The combination of the synergistic effect between Ni and Fe with the structural properties of the hybrid results in an efficient catalyst that generates a current density of 10 mA cm−2 at an overpotential of 240 mV, and also in a stable catalyst that operates continuously at low overpotentials for 160 h. KW - Water oxydation catalysis KW - EXAFS PY - 2017 DO - https://doi.org/10.1002/adfm.201703158 SN - 1616-301X SN - 1616-3028 VL - 27 IS - 40 SP - Article 1703158, 1 EP - 11 PB - WILEY-VCH Verlag CY - Weinheim AN - OPUS4-42783 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zhang, Luman A1 - de Greef, Nils A1 - Kalinka, Gerhard A1 - Van Bilzen, Bart A1 - Locquet, Jean-Pierre A1 - Verpoest, Ignaas A1 - Won Seo, Jin T1 - Carbon nanotube-grafted carbon fiber polymer composites: Damage characterization on the micro scale JF - Composites Part B N2 - Multiwall carbon nanotubes (CNTs) e carbon fibers (CFs)hybrid materials were produced by directly growing CNTs on CFs by means of chemical vapor deposition. For the latter, the oxidative dehydrogenation reaction of C2H2 and CO2 was applied, which allows growing CNTs without damaging the CF surface. Uni-directional nano-engineered carbon fiber reinforced composites (nFRCs) were fabricated by impregnating these hybrid materials with epoxy. The nFRCs subjected to single fiber push-out tests revealed a decrease of the interfacial shear strength (IFSS) of about 36% compared to the carbon fiber composites without CNTs. By means of transverse three-point bending tests performed on pre-notched composite beams inside a scanning electron microscope, the fracturing behavior parallel to the fibers was studied in-situ. The nFRCs showed significantly reduced fiber/matrix debonding while CNTs pull-out, CNTs bridging as well as matrix failure occurred. These results demonstrate that the presence of CNTs in nFRCs affects the stress distribution and consequently the damage Initiation as well as the damage propagation. The presence of CNTs suppresses the stress concentration at the fiber/Matrix interface and reduces the debonding of CFs from the matrix. However, our results indicate that the stress concentration shifts towards the CNTs' ends/matrix interface and causes promoted matrix failure leading to lower IFSS. KW - Carbon fibres nanotubes interface PY - 2017 DO - https://doi.org/10.1016/j.compositesb.2017.06.004 SN - 1359-8368 SN - 1879-1069 VL - 126 SP - 202 EP - 210 PB - Elsevier CY - Niederlande AN - OPUS4-42202 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Zhang, Lei T1 - Microstructure-property relationship in microalloyed high-strength steel welds N2 - Hochfeste Stähle sind bevorzugte Werkstoffe für die Herstellung von sicheren und zuverlässigen Strukturen in der Industrie. Dabei ist das Schmelzschweißen die Hauptverbindungstechnologie für diese Werkstoffgruppe. Während der Entwicklung der hochfesten niedriglegierten (engl. HSLA) Stähle wurden in der Vergangenheit unterschiedliche Legierungskonzepte mit fortgeschrittenen Herstellungstechniken kombiniert und umfassend untersucht. Jedoch befassten sich nur wenige Studien damit, wie die unterschiedliche Zusammensetzung der Legierungen die Eigenschaften der hochfesten Schweißverbindungen dieser Stähle beeinflussen, selbst im Fall begrenzter Gehalte von Mikrolegierungselementen. In der Schweißpraxis dieser hochfesten Stähle sind die Herausforderungen an die sich ausbildenden Mikrostruktur und den resultierenden mechanischen Eigenschaften von sehr großem Interesse. Diesbezüglich liegt der Hauptfokus des Interesses beim Einfluss der Mikrolegierungselemente auf die Phasenumwandlung sowie die resultierende Performance der Schweißverbindung selbst. Geringes Erweichen (Softening) der Wärmeeinflusszone (WEZ) sowie ein begrenztes Austenitkörner-Wachstum sind dabei erwünschte Eigenschaften der Schweißnaht, jedoch liegt das Hauptaugenmerk auf der Sicherstellung hervorragender Zähigkeits- und Zugeigenschaften. Zum Erreichen dieses Zieles werden Mikrolegierungselemente wie Ti, Nb oder V bewusst zu diesen modernen hochfesten Stählen zulegiert. Der Fokus der vorliegenden Arbeit ist das Verständnis, wie die mechanischen Eigenschaften der Verbindungen dieser HSLA-Stähle von Unterschieden in den jeweiligen Legierungskonzepten abhängen, die durch moderne Schweißprozesse gefügt werden. Zunächst wurden dazu drei unterschiedlich mikrolegierte (Nb, Ti und Ti+V Zugabe) Stähle vom Typ S690QL untersucht. Lichtmikroskopische Untersuchungen bestätigten dabei, dass eine ähnliche Zusammensetzung aus angelassenem Bainit und Martensit in allen drei Grundwerkstoffen vorherrschte und unterschiedlich stark vergröberte Ausscheidungen der Mikrolegierungselemente beobachtet wurden. Diese Ausscheidungen wurden weiterführend mittels thermodynamischer Softwareberechnung analysiert und durch Transmissions-Elektronen-Mikroskopie (TEM) identifiziert. Die Ergebnisse der mechanischen Werkstoffprüfung zeigten, dass alle drei Stähle oberhalb der nach Norm geforderten Zähigkeits- und Zugfestigkeitswerte lagen, jedoch Unterschiede im Dehnungsverhalten aufwiesen. Die drei Stähle wurden dann anschließend unter Verwendung des gleichen Schweißzusatzes geschweißt. Dabei wurde das abgeschmolzene Schweißgut durch die Mikrolegierungselemente aus dem Grundwerkstoff infolge der hohen Aufmischung beeinflusst. Die erhöhte Aufmischung bildet dabei ein wesentliches Merkmal der verwendeten modifizierten Sprühlichtbogentechnik. Als Ergebnis zeigte der Nb-mikrolegierte Stahl eine genügend hohe Aufnahme von Legierungselementen aus dem Grundwerkstoff in das Schweißgut, um dessen Mikrostruktur im Fall steigender Abkühlraten von nadeligem Ferrit hin zu Bainit zu verändern. Dieses wiederum reduzierte die Zähigkeitseigenschaften des Schweißgutes dieses Nb-legierten Stahls. Dieses Verhalten wurde in den beiden anderen Stählen nicht beobachtet. Ein zweiter Hauptpunkt dieser Arbeit war die Ausbildung der Mikrostruktur in der Feinkorn- und Grobkorn-WEZ und deren Zähigkeitseigenschaften mit den sich verändernden Schweißparametern. Zu diesem Zweck wurden definierte Werkstoffzustände physikalisch simuliert, um die resultierende Mikrostruktur sowie das Austenitkorn-Wachstum zu charakterisieren. Die Mikrolegierungselemente bildeten dabei einen wesentlichen Faktor zur Begrenzung des Austenitkörner-Wachstums. Das Ausmaß der Austenit-Vergröberung in der WEZ war dabei stark abhängig von der Art und dem Volumenanteil der unterschiedlichen Ausscheidungen infolge der unterschiedlichen Mikrolegierung. Von allen dreiStählen zeigte die WEZ des Ti-legierten Grundwerkstoffes das geringste Kornwachstum als Folge des ausreichenden Umfangs von stabilen Ti-Ausscheidungen. Die Ausbildung von nadeligem Ferrit im Korn wurde dabei durch die Ti-Ausscheidungen unterstützt, da diese als bevorzugte Stellen der Nukleation des Ferrits dienten. Die Zähigkeit der WEZ erhöhte sich dabei infolge der Großwinkelgrenzen der feinen Ferrit-Platten. Aufgrund des kombinierten Effektes von Nb und Mo, welcher sich in der bevorzugten Ausbildung von unterem Bainit äußert, konnte die WEZ-Zähigkeit bei hohen Abkühlraten weiter verbessert werden. Im Fall eines größeren Wärmeeintrags bildete sich jedoch bevorzugt oberer Bainit, welcher wiederum die Zähigkeit reduzierte. Der abschließende experimentelle Teil der Arbeit konzentrierte sich auf das Verständnis der Mechanismen, die in bestimmten Fällen zur Erweichung (oder Softening) der WEZ führen. Dieses Erweichen äußerte sich in den unterschiedlichen Zugeigenschaften der geschweißten Verbindungen der Stähle. Dabei war die Bruchlage entweder in der erweichten WEZ oder im Grundwerkstoff, abhängig von den Schweißparametern sowie der Art des geschweißten Stahls. Im Ti-legierten Stahl führte dabei ein erhöhter Wärmeeintrag zur Vergrößerung der Erweichungszone. Dieses führte zu einer signifikanten Abnahme der Härte und anschließend zum Versagen in dieser erweichten Zone im Zugversuch. Die Veränderung der Bruchlage hin zum Grundwerkstoff wurde durch die Begrenzung des Wärmeintrags erreicht. Dieses Verhalten wurde nicht in den beiden anderen Stählen beobachtet. Dieses Verhalten zeigt, dass bereits kleine Unterschiede im Gehalt der Mikrolegierungselemente der Stähle zu großen Variationen in den Zugeigenschaften führten. Für alle drei Stähle, zeigten die Ti-enthaltenden Schweißverbindungen das am deutlichsten ausgeprägte Softening, gefolgt von den Ti+V-enthaltenden Schweißungen und schließlich den Nb-enthaltenden Schweißverbindungen. Das unterschiedliche Softening konnte dabei auf zwei Prozesse bezogen werden, die auch über zusätzliche Dilatometrie-Experimente gestützt wurden: die Phasenumwandlung und das Anlassverhalten. Im Ti-legiertem Stahl lag nach der Phasenumwandlung großformatiger Ferrit als Konsequenz der ursprünglich großen Austenitkörner vor. Dieses führte zu einer abgesenkten Härte dieses Stahls. Weiterhin resultierte die geringere Anlassbeständigkeit des Ti-legierten Stahls (gegenüber dem Nb-legierten Stahl) zu einem weiteren Softening der erweichten WEZ. Deswegen erwies sich diese Kombination aus Legierungszusammensetzung und Schweißwärmeeintrag als kritisch, gestützt durch die Experimente am gleichen S690QL Stahl. Die vorliegende Arbeit hebt den wesentlichen Einfluss der Mikrolegierungselemente auf die Schweißmikrostrukturen und die mechanischen Eigenschaften der Schweißverbindungen hervor. Die Kenntnis dieser empfindlichen Balance zwischen Legierungskonzept des entsprechenden Stahls und geeigneten Schweißparametern ist als kritisch für das fertige Produkt anzusehen. Dazu stellt diese Arbeit spezifische Empfehlungen und Ergebnisse zur Verfügung, um die korrekte Schweißpraxis zu gewährleisten als auch für die Zusammensetzung mikrolegierter hochfester Stähle. N2 - High-strength steels are favoured materials in the industry for production of safe and sustainable structures. The main technology used for joining the components of such steel is fusion welding. Steel alloy design concepts combined with advanced processing technologies have been extensively investigated during the development of High-Strength Low-Alloy (HSLA) steels. However, very few studies have addressed the issue of how various alloy designs, even with limited microalloy addition, can influence the properties of high-strength steel welds. In high-strength steel welding practices, the challenges regarding microstructure evolution and the resulting mechanical properties variation, are of great interest. The main focus is the debate regarding the role of microalloy elements on phase transformation and weld performance. Limited Heat Affected Zone (HAZ) softening and limited austenite grain coarsening are significant design essentials, but the primary goal is to ensure excellent toughness and tensile properties in the steel weld. To achieve this purpose, microalloy elements such as Ti, Nb, or V were intentionally added to modern high-strength steels. The focus of this work was to understand the mechanical properties of HSLA steels resulting from differences in alloy design after joining by modern welding processes. To begin, three microalloyed S690QL steels (Nb, Ti, and Ti+V addition) were investigated. Optical microscopy confirmed that similar mixtures of tempered bainite and martensite predominated the parent microstructure in the three steels, different types of coarse microalloy precipitates were also visible. These precipitates were analysed by using a thermodynamic-based software and then identified by Transmission Electron Microscopy (TEM). Results of mechanical testing revealed that all three steels performed above the standard toughness and tensile strength values, but with varied yielding phenomena. During the welding operation, each of the three steels was joined by using the same filler material. The fused weld metal was influenced by the high dilution of microalloyed elements in the base metal, this was significantly pronounced during the modified spray arc welding technique. As a result, the Nb-containing steel exhibited sufficient amounts of alloy pick-up to transition the microstructure in the weld metal from acicular ferrite to bainite as cooling rate was increased, leading to reduced toughness. This was not observed with the other two steels. A second focus was made on the microstructure Evolution and toughness properties of the coarse and fine grained HAZ as welding parameters changed. In order to characterise the microstructure and austenite grain growth behaviour, physical simulations were conducted. The microalloy precipitates were found to be a dominant factor restricting the austenite grain coarsening. The extent of Austenite coarsening in the HAZ is closely related to the type and volume fraction of each microalloy precipitate. Among the three steels, the Ti-containing HAZ exhibited the smallest extent of grain growth due to the sufficient amount of stable Ti-rich precipitates. Microalloy Addition also markedly influenced the subsequent phase transformation in the HAZ. The formation of intragranular acicular ferrite was promoted by Ti-rich precipitate, acting as favourable nucleation sites of ferrite. This structure enhanced the HAZ toughness owing to fine, high-angle boundaries of ferrite plates. The synergistic effect of Nb and Mo elements was beneficial to improve the HAZ toughness at fast cooling rates by promoting fine lower bainite formation. At high heat input, large upper bainite was formed which caused reduced toughness. The final set of experimental work was concentrated on understanding the HAZ softening mechanisms that influenced variations in the tensile properties of the welded joints. The tensile failure in the softened HAZ or base material depended on the welding parameters and the type of steel being joined. In Ti-containing steel, increased heat Input extended the softened zone width, which caused a significant decrease in hardness and then resulted in failure in this area. Therefore, limited heat Input was used to shift failure position to base material. But this was not observed in the other two steels. Hence, small differences in microalloy addition exhibited large variation in tensile properties. Among the three steels, Ti-containing welds were found to have the most pronounced softening, followed by Ti+V-containing welds and finally Nb-containing welds. This varied softening phenomenon was related to two significant processes supported by the results of additional dilatometry simulation: phase transformation and tempering behaviour. In the Ti-containing steel, the phase Transformation product ferrite was large-sized, as a consequence of initial large austenite grains. This led to the decreased corresponding hardness of the Ti-containing steel. Furthermore, lower tempering resistance in Ti-containing steel as compared to Nb-containing steel, resulted in additional softening effect in the softened HAZ. Therefore, steel alloy identification and heat Input during welding were critical, proven by the experimentation within the same S690QL steel grade. This work emphasised the influence of microalloy elements on weld microstructure and mechanical properties in welded joints. Knowledge of this delicate balance between steel alloy design and appropriate welding parameters is critical for the end product. Thus, this work provides specific recommendations and results to ensure proper welding practice and steel design of microalloyed high-strength steels. T3 - BAM Dissertationsreihe - 155 KW - Microalloyed steel KW - Weld microstructure KW - HAZ softening KW - Mechanical properties PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-391574 SN - 978-3-9818270-4-0 SN - 1613-4249 VL - 155 SP - 1 EP - 183 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-39157 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zeegers, G. P. A1 - Steinhoff, R. F. A1 - Weidner, Steffen A1 - Zenobi, R. T1 - Evidence for laser-induced redox reactions in matrix-assisted laserdesorption/ionization between cationizing agents and target plate material: a study with polystyrene and trifluoroacetate salts JF - International Journal of Mass Spectrometry N2 - Matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) is often applied to assess the dispersity and the end groups of synthetic polymers through the addition of cationizing agents. Here weaddress how these cation adducts are formed using polystyrene (PS) as a model polymer. We analyzed PSby MALDI-MS with a 2-[(2E)-3-(4-tert-butylphenyl)-2-methylprop-2-enylidene]malononitrile (DCTB) as the matrix and a range of trifluoroacetate (TFA) salts as cationizing agents on a range of different targetplate materials (copper, 1.4301 stainless steel, aluminum, Inconel 625, Ti90/Al6/V4 and chromium-, gold-and silver-plated stainless steel). It was found that on a stainless steel substrate the metal cations Al+,Li+, Na+, Cu+and Ag+formed polystyrene adducts, whereas K+, Cs+, Ba2+, Cr3+, Pd2+, In3+, or their lower oxidation states, did not. For the copper and silver substrates, PS and DCTB adduct formation with cations liberated from these target plate materials was observed upon addition of a cationizing agent, which indicates the occurrence of redox reactions between the added TFA salts and the target plate material. Judging from their standard electrode potentials, these redox reactions would not normally occur, i.e.,they require an additional energy input, strongly suggesting that the observed redox reactions are laser-induced. Furthermore, copper granules were found to successfully sequester PS from a tetrahydrofuran(THF) solution, consistent with the view complex formation with the copper target plate can take place prior to the MALDI-MS measurement. KW - Polymer MALDI KW - Cationization KW - Polystyrene KW - Laser-induced redox reactions KW - Target plate material PY - 2017 DO - https://doi.org/10.1016/j.ijms.2016.10.007 SN - 1387-3806 SN - 1873-2798 VL - 416 SP - 80 EP - 89 PB - Elsevier B.V. AN - OPUS4-41146 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - You, Zengchao A1 - Weidner, Steffen A1 - Jakubowski, Norbert A1 - Meermann, Björn A1 - Panne, Ulrich T1 - Nanoparticles separation using capillary electrophoresis N2 - A common method for nanoparticle separation, which was introduced in 1976 by Giddings, represents asymmetrical field-flow fractionation (AF4). It is a flow based separation method, which can be theoretically used to separate particles range from 1 nm to 50 µm. However, when the particles are smaller than 10 nm, separation with AF4 will become difficult to perform. Because in this case strong separation force, which induces aggregation of particles, should be applied. This will decrease recoveries of analytes and limit its application in accurate quantitative analysis. Capillary electrophoresis (CE) is another well-developed separation technique, in which samples will be separated in relation to their electrophoretic mobility. In recent years, CE has been used to separate different kinds of nanoparticles like, gold colloids or CdSe Quantum dots. However, till now only separation of particles smaller than 50 nm was reported. Because large size distribution of bigger particles will result in strong peak broadening and long separation time. A two-dimensional coupling of AF4 and CE might provide us a new separation method, which can extend the separation ranges of both methods and be a way to characterise particles with large size distributions. T2 - BAM PhD seminar CY - PhD seminar, Berlin, Germany DA - 23.06.2017 KW - Nanoparticles separation capillary electrophoresis asymmetrcial flow field flow fractionation PY - 2017 AN - OPUS4-47186 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Yilmaz, M. A1 - Wollschläger, Nicole A1 - Esfahani, M. N. A1 - Österle, Werner A1 - Leblebici, Y. A1 - Alaca, B. E. T1 - Superplastic behavior of silica nanowires obtained by direct patterning of silsesquioxane-based precursors JF - Nanotechnology N2 - Silica nanowires spanning 10 μm-deep trenches are fabricated from different types of silsesquioxane-based precursors by direct e-beam patterning on silicon followed by release through deep reactive ion etching. Nanowire aspect ratios as large as 150 are achieved with a critical dimension of about 50 nm and nearly rectangular cross-sections. In situ bending tests are carried out inside a scanning electron microscope, where the etch depth of 10 mm provides sufficient space for deformation. Silica NWs are indeed observed to exhibit superplastic behavior without fracture with deflections reaching the full etch depth, about two orders of magnitude larger than the nanowire thickness. A large-deformation elastic bending model is utilized for predicting the deviation from the elastic behavior. The results of forty different tests indicate a critical stress level of 0.1–0.4 GPa for the onset of plasticity. The study hints at the possibility of fabricating silica nanowires in a monolithic Fashion through direct e-beam patterning of silsesquioxane-based resins. The fabrication technology is compatible with semiconductor manufacturing and provides silica nanowires with a very good structural integrity. KW - Silica nanowires KW - HSQ KW - Superplasticity KW - In situ bending tests PY - 2017 DO - https://doi.org/10.1088/1361-6528/aa5b80 SN - 0957-4484 SN - 1361-6528 VL - 28 IS - 11 SP - Article 115302, 1 EP - 10 AN - OPUS4-39166 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Yilmaz, M. A1 - Kilinc, Y. A1 - Nadar, G. A1 - Tasdemir, Z. A1 - Wollschläger, Nicole A1 - Österle, Werner A1 - Leblebici, Y. A1 - Alaca, B. E. T1 - Top-down technique for scaling to nano in silicon MEMS JF - Journal of Vacuum Science & Technology B, Nanotechnology and Microelectronics: Materials, Processing, Measurement, and Phenomena N2 - Nanoscale building blocks impart added functionalities to microelectromechanical systems (MEMS). The integration of silicon nanowires with MEMS-based sensors leading to miniaturization with improved sensitivity and higher noise immunity is one example highlighting the advantages of this multiscale approach. The accelerated pace of research in this area gives rise to an urgent need for batch-compatible solutions for scaling to nano. To address this challenge, a monolithic fabrication approach of silicon nanowires with 10-lm-thick silicon-on-insulator (SOI) MEMS is developed in this work. A two-step Si etching approach is adopted, where the first step creates a shallow surface protrusion and the second step releases it in the form of a nanowire. It is during this second deep etching step that MEMS—with at least a 2-order-of-magnitude scale difference - is formed as well. The technique provides a pathway for preserving the lithographic resolution and transforming it into a very high mechanical precision in the assembly of micro- and nanoscales with an extreme topography. Validation of the success of integration is carried out via in situ actuation of MEMS inside an electron microscope loading the nanowire up to its fracture. The technique yields nanowires on the top surface of MEMS, thereby providing ease of access for the purposes of carrying out surface processes such as doping and contact formation as well as in situ observation. As the first study demonstrating such monolithic integration in thick SOI, the work presents a pathway for scaling down to nano for future MEMS combining multiple scales. KW - Nanowires KW - Silicon KW - Top-down KW - MEMS PY - 2017 DO - https://doi.org/10.1116/1.4978047 SN - 1071-1023 VL - 35 IS - 2 SP - 022001-1 EP - 022001-7 PB - America Vacuum Society AN - OPUS4-39370 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Yildirim, Arda A1 - Sentker, K. A1 - Huber, P. A1 - Schönhals, Andreas T1 - Structure, Dynamics and Phase Behavior of a Discotic Liquid Crystal Confined in Nanoporous Anodic Aluminum Oxide Membranes N2 - The interest in porous anodic aluminum oxide (AAO) has been rapidly growing due to its numerous applications in separation, catalysis, energy generation and storage, electronics, and sensors. From the scientific point of view, AAO is a topical interest in soft matter fields. Spatial confinement of soft matter in nanoporous media influences its structure, thermodynamics, and mobility. Embedding polymers and liquid crystals into nanopores of AAO results in a 2D nanoconfinement of these materials. This confinement affects their properties, compared to the bulk, such as phase transition temperatures and enthalpies, molecular mobility, and architecture of the crystallization. On the other hand, discotic liquid crystals (DLCs) are a promising class of soft matter for electronic applications. This is due to their ability to organize and stack themselves into columns in a hexagonal columnar mesophase, a mesophase in between the plastic crystalline and isotropic phase, driven by the overlap of the π orbitals of their aromatic core. This leads to a high charge-carrier mobility along the column axis. Further, these columns could then be considered as “molecular nanowires”. In this study, 2,3,6,7,10,11 hexakis[hexyloxy] triphenylene (HAT6), a triphenylene based DLC, was confined into nanoporous AAO membranes. The structure, dynamics and the phase behavior of the confined HAT6 were investigated by broadband dielectric spectroscopy (BDS) and differential scanning calorimetry (DSC). HAT6 was embedded into nanoporous AAO membranes by melt infiltration in the isotropic phase under argon atmosphere. The membranes have parallel aligned cylindrical nanopores, with pore diameter of 10, 20, 25, 40, 80, 120 and 180 nm. The filling degree for each sample was checked by thermogravimetric analysis (TGA) in order to ensure complete filling. Bulk HAT6 forms a hexagonal columnar phase; in between the isotropic phase above 371 K and the plastic crystalline phase below 340 K. Unlike the bulk, the confined HAT6 split the plastic crystalline-to-hexagonal columnar phase transition in two, which might be interpret as two different phase structures; close to the wall and at the pore center. Moreover, the isotropic-to-columnar transition of the confined HAT6 shifted, with decreasing pore diameter, to lower temperatures. Furthermore, pore surfaces of a series of membranes were chemically modified, resulting in a more hydrophobic pore surface than the unmodified ones. HAT6 was embedded into the modified membranes by the same aforementioned preparation. The influence of the changed host-guest-interaction, on the structure, dynamics, and the phase behavior of HAT6 confined in the modified membranes, was also investigated by BDS and DSC. T2 - 9th International Conference on Porous Media & Annual Meeting CY - Rotterdam, The Netherlands DA - 08.05.2017 KW - Nanoporous media KW - Anodic Aluminum Oxide KW - Discotic Liquid Crystal PY - 2017 AN - OPUS4-40089 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Yildirim, Arda A1 - Sentker, K. A1 - Huber, P. A1 - Schönhals, Andreas T1 - Structure, Dynamics and Phase Behavior of a Discotic Liquid Crystal Confined in Nanoporous Anodic Aluminum Oxide Membranes N2 - Discotic liquid crystals (DLCs) are a promising class of soft matter for electronic applications. This is due to their ability to organize and stack themselves into columns in a hexagonal columnar mesophase, driven by the overlapping of the π orbitals of their aromatic core. This leads to a high charge-carrier mobility along the column axis. Previous studies on DLCs showed that their properties, such as phase transition temperatures and enthalpies, are susceptible to nanoconfinement. In this study, 2,3,6,7,10,11 hexakis[hexyloxy] triphenylene (HAT6), a triphenylene based DLC, was confined into parallel aligned cylindrical nanopores of anodic aluminum oxide (AAO) membranes by melt infiltration in the isotropic phase under an argon atmosphere. Furthermore, the pore surfaces of a series of membranes were chemically modified, resulting in a more hydrophobic pore surface than the unmodified ones. The structure, dynamics, and the phase behavior of HAT6 confined into modified and unmodfied nanopores of AAO were investigated by broadband dielectric spectroscopy and differential scanning calorimetry. Results will be discussed in detail. T2 - DPG Spring Meeting 2017 CY - Dresden, Germany DA - 19.03.2017 KW - Discotic Liquid Crystals KW - Nanoconfinement PY - 2017 AN - OPUS4-39561 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Yildirim, Arda A1 - Sentker, K. A1 - Huber, P. A1 - Schönhals, Andreas T1 - Structure, Dynamics and Phase Behavior of a Discotic Liquid Crystal Confined in Nanoporous Anodic Aluminum Oxide Membranes N2 - Discotic liquid crystals (DLCs) are a promising class of soft matter for electronic applications. This is due to their ability to organize and stack themselves into columns in a hexagonal columnar mesophase, a mesophase in between the plastic crystalline and isotropic phase, driven by the overlap of the π orbitals of their aromatic core. This leads to a high charge-carrier mobility along the column axis. Further, these columns could then be considered as “molecular nanowires”. Spatial confinement of soft matter in nanoporous media influences its structure, thermodynamic properties, and mobility. Embedding liquid crystals and polymers into nanopores of anodic aluminum oxide (AAO) results in a 2D nanoconfinement of these materials. This confinement affects their properties, compared to the bulk, such as phase transition temperatures and enthalpies, molecular mobility, and architecture of the crystallization. In this study, 2,3,6,7,10,11 hexakis[hexyloxy] triphenylene (HAT6), a triphenylene-based DLC, was confined into nanoporous AAO membranes. The structure, dynamics and the phase behavior of the confined HAT6 were investigated by broadband dielectric spectroscopy (BDS) and differential scanning calorimetry (DSC). HAT6 was embedded into nanoporous AAO membranes by melt infiltration in the isotropic phase under argon atmosphere. The membranes have parallel aligned cylindrical nanopores, with different pore diameters in the range of 10-180 nm. Bulk HAT6 forms a hexagonal columnar phase; in between the isotropic phase above 371 K and the plastic crystalline phase below 340 K. Unlike the bulk, the confined HAT6 split the phase transitions in two or more, which might be interpret as different phase structures; close to the wall and at the pore center. Moreover, the phase transitions of the confined HAT6 shifted, with decreasing pore diameter, to lower temperatures. The dependencies of the phase transition temperatures on the pore size was well-described by the Landau-de Gennes model. Furthermore, pore surfaces of a series of membranes were chemically modified, resulting in a more hydrophobic pore surface than the unmodified ones. HAT6 was embedded into the modified membranes by the same aforementioned preparation. The influence of the changed host-guest-interaction, on the structure, dynamics, and the phase behavior of HAT6 confined in the modified membranes, was also investigated by BDS and DSC. T2 - Liquids 2017 – 10. Liquid Matter Conference CY - Ljubljana, Slovenia DA - 17.07.2017 KW - Discotic Liquid Crystals KW - Nanoconfinement PY - 2017 AN - OPUS4-41178 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Yildirim, Arda T1 - Structure, Dynamics and Phase behavior of bulk and confined liquid crystals N2 - In this study, the molecular dynamics of two linear-shaped tetramethylated guanidinium triflates ionic liquid crystals were investigated by a combination of Broadband Dielectric Spectroscopy (BDS) and Specific Heat Spectroscopy (SHS). Three processes were detected by BDS; at low temperature γ-process, at higher temperatures α-process and at even higher temperatures conductivity. The γ-process indicates localized fluctuations, and the α-process designates cooperative fluctuations. Slightly different restrictions were found for conductivity processes of LC536 and LC537 due to the slightly different lengths of alky chains. Furthermore, the cooperative dynamics were also probed by SHS. The cooperative dynamics probed by the different techniques (BDS and SHS) compared, and assigned to the different restrictions on the cooperativity due to the difference in the sensitivity of the techniques. T2 - Seminar Vortrag Universität Stuttgart CY - Stuttgart, Germany DA - 24.07.2017 KW - Discotic Liquid Crystals PY - 2017 AN - OPUS4-41179 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Würth, Christian A1 - Kaiser, Martin A1 - Wilhelm, Stefan A1 - Grauel, Bettina A1 - Hirsch, Th. A1 - Resch-Genger, Ute T1 - Excitation power dependent population pathways and absolute quantum yields of upconversion nanoparticles in different solvents JF - Nanoscale N2 - The rational design of brighter upconversion nanoparticles (UCNPs) requires a better understanding of the radiationless deactivation pathways in these materials. Here, we demonstrate the potential of excitation power density (P)-dependent studies of upconversion (UC) luminescence intensities, slope factors, and absolute quantum yields (ΦUC) of popular β-NaYF4:20% Yb3+,2% Er3+ UCNPs of different surface chemistries in organic solvents, D2O, and water as a tool to gain deeper insight into the UC mechanism including population and deactivation pathways particularly of the red emission. Our measurements, covering a P regime of three orders of magnitude, reveal a strong difference of the P-dependence of the ratio of the green and red luminescence bands (Ig/r) in water and organic solvents and P-dependent population pathways of the different emissive energy levels of Er3+. In summary, we provide experimental evidence for three photon processes in UCNPs, particularly for the red emission. Moreover, we demonstrate changes in the excited population dynamics via bi- and triphotonic processes dependent on the environment, surface chemistry, and P, and validate our findings theoretically KW - Upconverion KW - Quantum Yield KW - Photo physics PY - 2017 UR - http://pubs.rsc.org/en/content/articlepdf/2017/nr/c7nr00092h DO - https://doi.org/10.1039/c7nr00092h SN - 2040-3364 SN - 2040-3372 VL - 9 IS - 12 SP - 4283 EP - 4294 PB - The Royal Society of Chemistry AN - OPUS4-39849 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Würth, Christian A1 - Kaiser, Martin A1 - Resch-Genger, Ute T1 - New Trends in Fluorometry - Fluorescence Measurements above 1000 nm N2 - Trends in fluorometry and fluorescence imaging are increasing applications of molecular and nanoscale reporters with emission > 800 nm and recently also > 1000 nm for bioanalysis, medical diagnostics, bioimaging, and safety barcodes. Mandatory for the comparison of different emitter classes and the rational design of the next generation of reporters for the short wavelength infrared (SWIR) region are reliable and quantitative photoluminescence measurements in this challenging wavelength region. This is of special relevance for nanocrystalline emitters like semiconductor quantum dots and rods as well as lanthanide-based upconversion and downconversion nanocrystals, where surface states and the accessibility of emissive states by quenchers largely control accomplishable photoluminescence quantum yields and hence, signal sizes and detection sensitivities from the reporter side. Such measurements are currently hampered by the lack of suitable methods and standards for instrument calibration and validation and quantum yield standards with emission > 800 nm and especially > 1000 nm. In this respect, we present the design of integrating sphere setups for absolute and excitation power density-dependent measurements of emission spectra and photoluminescence quantum yields in the wavelength region of 650 to 1650 nm including calibration strategies and first candidates for potential fluorescence standards. Subsequently, selected examples for spectroscopic studies of different types of nanocrystals are presented including the upconversion and downconversion emission of differently sized and surface functionalized lanthanide-doped nanoparticles T2 - COSP-Colloquium Optical Spectroscopy CY - Berlin, Germany DA - 27.11.2017 KW - Yield KW - IR fluorescence KW - Quantum dot KW - Upconversion nanocrystal KW - Lanthanide emitter KW - NIR KW - Integrating sphere spectroscopy KW - Absolute fluorescence quantum PY - 2017 AN - OPUS4-43327 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Würth, Christian A1 - Kaiser, M. A1 - Levchuk, I. A1 - Batentschuk, M. A1 - Hirsch, T. A1 - Resch-Genger, Ute T1 - Absolute quantum yield measurements of spectral conversion materials - Instrumentation and applications N2 - The direct measure for the conversion efficiency of absorbed photons into emitted light by an emissive species or chromophore is the photoluminescence quantum yield (pl).1 pl is the fluorometric key quantity that controls the suitability of a molecule or material e.g. for application as a label, probe or sensor molecule or as a converter material. A straightforward approach to pl values presents their absolute determination using an integrating sphere set up. This procedure circumvents the use of standards thereby avoiding additional measurements and uncertainties related to their often debated pl values. In this respect, we discuss the experimental requirements on absolute measurements of down and upconversion quantum yields (UC), the later presents currently one of the most challenging spectroscopic measurements due to its multiphotonic character. We explore the challenges for determination of excitation power density (P) dependent pl(P), present the design and characterization of a unique integrating sphere setup for such measurements in the vis to IR spectral region including its calibration, and the influence of the excitation beam profile to perform pl measurements of liquid and solid materials. As an example for downshifting materials we present doped core-shell CdSe/ZnS semiconductor quantum dots (d-dots) which show a nearly host material and crystal size independent emission with large Stokes shifts and minimum reabsorption.2 Systematic variation of the reaction components, parameters and thickness of the ZnS shell yielded doped nanocrystals with a very high pl, high reproducibility and large quantities. Application of these NCs in the light conversion layers of commercial monocrystalline silicon (mono-Si) solar cells led to a significant enhancement of the external quantum efficiency (EQE) of this devices in the ultraviolet spectral region between 300 and 400 nm. On the other hand, lanthanide-doped up-converting nanoparticles (UCNPs), are promising light converters from the near infrared to the visible region. These NPs show multiple narrow emission bands in the visible (vis) and NIR, excellent photostability, and long luminescence lifetimes. The rational design of brighter UCNP requires an improved understanding of the radiationless deactivation pathways, that are affected by size, surface chemistry, and microenvironment.3 We give an insight into the influences of these parameters on the photophysical key characteristics of the upconversion process such as UC(P), the luminescence decay behavior, the power dependent red-to-green intensity ratio, and intensities of the individual emission bands. T2 - MCare-Materials Challenges in Alternative and Renewable Energy CY - Jeju, Korea DA - 20.02.2017 KW - Energy conversion KW - Quantum yield KW - Doped quantum dots KW - Upconversion PY - 2017 AN - OPUS4-40009 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Würth, Christian A1 - Kaiser, M. A1 - Resch-Genger, Ute T1 - Theory of quantum yields - Excitation power dependent measurements N2 - Introduction to power dependent QY-measurements and upconversion T2 - Cost-action Training school CY - Turku, Finland DA - 03.04.2017 KW - Quantum yield KW - Upconversion PY - 2017 AN - OPUS4-40011 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wäsche, Rolf A1 - Steinborn, Gabriele A1 - Woydt, Mathias T1 - Colloidal processing of metal bonded niobium carbide T2 - International Conference on Refractory Metals and Hard Materials N2 - Manufacturing of Niobium carbide cermets with nickel binder and different additions of titanium carbide has been realized by colloidal processing in aqueous environment. T2 - 19. Plansee Seminar CY - Reutte, Austria DA - 29.05.2017 KW - NbC KW - TiC KW - Ni KW - Colloidal processing KW - Gas pressure sintering KW - Hardness PY - 2017 SP - HM 135/1 EP - HM 135/11 AN - OPUS4-40596 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -