TY - GEN A1 - Hasenstab, Andreas A1 - Hillemeier, B. A1 - Krause, Martin ED - Bröker, F. T1 - Defect localisation in wood with low frequency ultrasonic echo technique T2 - 14th International Symposium on Nondestructive Testing of Wood CY - Eberswalde, Germany DA - 2005-05-02 PY - 2005 SN - 3-8322-3949-9 SP - 331 EP - 336 PB - Shaker CY - Aachen AN - OPUS4-11307 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Martin, Sven A1 - Krüger, Jörg A1 - Hertwig, Andreas A1 - Fiedler, A. A1 - Kautek, Wolfgang T1 - Femtosecond laser interaction with protection materials N2 - Textile, aluminium and polyethylene used as components in laser protection curtains were investigated with respect to their ablation behaviour. Employing 33-fs pulses (800 nm wavelength, 1 kHz repetition rate), ex situ geometrical measurements of the ablation cavities and in situ acoustic investigations with a microphone were performed to determine the ablation thresholds in the single- and multi-pulse cases. The acoustical method proved advantageous for complex surface morphologies and/or single laser pulse interactions. Incubation phenomena can be observed for all the materials studied. Technically relevant multi-pulse ablation thresholds are presented and are compared with the single-pulse (1-on-1) irradiation. KW - Damage KW - Femtosecond laser ablation KW - Laser safety KW - Threshold KW - Aluminium KW - Textile PY - 2003 DO - https://doi.org/10.1016/S0169-4332(02)01392-2 SN - 0169-4332 SN - 1873-5584 VL - 208-209 SP - 333 EP - 339 PB - North-Holland CY - Amsterdam AN - OPUS4-11546 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bunte, J. A1 - Barcikowski, S. A1 - Burmester, T. A1 - Püster, T. A1 - Hertwig, Andreas A1 - Kautek, Wolfgang A1 - Krüger, Jörg A1 - Martin, Sven A1 - Spielmann, C. A1 - Lenner, M. A1 - Brose, M. T1 - Sicherer Umgang mit Ultrakurzpuls-Lasern, Teil 1: Primäre Gefährdungen PY - 2005 SN - 0945-8875 IS - 2 SP - 6 EP - 11 PB - Magazin-Verl. CY - Bad Nenndorf AN - OPUS4-11001 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bunte, J. A1 - Barcikowski, S. A1 - Burmester, T. A1 - Püster, T. A1 - Hertwig, Andreas A1 - Kautek, Wolfgang A1 - Krüger, Jörg A1 - Martin, Sven A1 - Spielmann, C. A1 - Lenner, M. A1 - Brose, M. T1 - Sicherer Umgang mit Ultrakurzpuls-Lasern, Teil 2: Sekundäre Gefährdungen PY - 2005 SN - 0945-8875 IS - 4 SP - 13 EP - 18 PB - Magazin-Verl. CY - Bad Nenndorf AN - OPUS4-11002 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hertwig, Andreas A1 - Martin, S. A1 - Kautek, Wolfgang A1 - Krüger, Jörg ED - Maruray, L. T1 - Ultra-short Pulse Laser Safety - a Challenge to Materials Science N2 - In this paper, safety-related experiments with ultra-short laser pulses (down to 30 fs) on various components (goggles, curtains) for laser protection are presented. The damage and failure behaviour of protective devices has been investigated dependent on practical conditions such as pulse duration, laser .uence, pulse number, and repetition rate. The e.ects of laser-irradiation on materials can be roughly divided into transient ones like laserinduced transmission (LIT) or short-lived colour centres and permanent damages like the stable colour centres and ablation. The former e.ects are particularly important for transparent devices like laser goggles. To obtain a complete overview on laser safety issues and the prevention of failure there are two important .elds of investigation: 1. the e.ects of laser radiation on human eyes and skin, and 2. on the possible protection materials. Both .elds have been addressed during the recently .nished German project SAFEST (safety aspects in femtosecond technology). The amount of safety data available in the ultrashort pulse region has been increased remarkably. This allows for a re-evaluation of known laser protection materials for this region of pulse durations and for the evaluation of new designs that promise high protection levels while being light-weight and convenient to use. T2 - Optical design and engineering II CY - Jena, Germany DA - 2005-09-13 PY - 2005 N1 - Serientitel: Proceedings of SPIE – Series title: Proceedings of SPIE IS - 5962 SP - 59622J-1 - 59622J-10 PB - SPIE CY - Bellingham AN - OPUS4-11593 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Hasenstab, Andreas A1 - Krause, Martin T1 - Ultraschall-Echo-Technik zur Ortung von Minderdicken und Schäden in Holzbauteilen T2 - DGZfP-Fachtagung Bauwerksdiagnose "Praktische Anwendungen Zerstörungsfreier Prüfungen" CY - Berlin, Deutschland DA - 2006-02-22 KW - Zerstörungsfreie Prüfung KW - Holz KW - Ultraschallecho KW - ZfP an Holzbauteilen KW - Fehlstellen KW - Minderdicken KW - Ultraschall-Echo KW - Fäulnis KW - Bauwesen PY - 2006 SN - 3-931381-71-4 SP - 1(?) EP - 11(?) PB - DGZfP CY - Berlin AN - OPUS4-14233 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hasenstab, Andreas A1 - Krause, Martin A1 - Osterloh, Kurt T1 - Testing Of Wooden Construction Elements with Ultrasonic Echo Technique and X-Ray T2 - 9th European Conference on NDT CY - Berlin, Germany DA - 2006-09-25 KW - NDT of Wood PY - 2006 SN - 3-931381-86-2 SP - 1(?) EP - 8(?) PB - European Federation for Non-Destructive Testing CY - Berlin AN - OPUS4-14422 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hao, Ning A1 - Böhning, Martin A1 - Goering, Harald A1 - Schönhals, Andreas T1 - Nanocomposites of Polyhedral Oligomeric Phenethylsilsesquioxanes and Poly(bisphenol A carbonate) as Investigated by Dielectric Spectroscopy N2 - Nanocomposites were prepared by solution blending of polyhedral oligomeric silsesquioxane with phenethyl substituents (PhenethylPOSS) into poly(bisphenol A carbonate) (PBAC). The nanocomposites were investigated by dielectric spectroscopy, differential scanning calorimetry (DSC) and density measurements. PhenethylPOSS shows one relaxation process, the α-relaxation, confirmed by DSC investigations. PBAC shows a β-relaxation at lower and an α-relaxation at higher temperatures. With increasing PhenethylPOSS content the α-relaxation of the composites shifts to lower temperatures. Thus, incorporation of PhenethylPOSS leads to a plasticization of PBAC due to a decrease of the packing density which is rationalized by density measurements. For higher concentrations of PhenethylPOSS (>10 wt %) the α-relaxation of the polycarbonate matrix splits into two peaks. Moreover, close to the α-relaxation of PhenethylPOSS a third process is observed. These results indicate a phase separation into a PBAC matrix with a few percents of molecularly solved POSS and POSS-rich domains. These POSS-rich domains are surrounded by an interfacial layer of PBAC having a higher concentration of POSS than the matrix. A phase diagram is deduced providing a miscibility criterion. For the phase separated nanocomposites an interfacial polarization phenomena is observed. Using a simplified model the time constant of this process is correlated with the size of the PhenethylPOSS-rich domains and theire increasing size with the increase of the concentration of POSS. KW - Polyhedral oligomeric silsesquioxane (POSS) KW - Polymer-based nanocomposites KW - Broadband dielectric spectroscopy KW - Interfacial polarisation PY - 2007 SN - 0024-9297 SN - 1520-5835 VL - 40 IS - 8 SP - 2955 EP - 2964 PB - American Chemical Society CY - Washington, DC AN - OPUS4-14768 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hao, Ning A1 - Böhning, Martin A1 - Schönhals, Andreas T1 - Gas Transport Properties of Polymeric Nanocomposites Based on Polyhedral Oligomeric Silsesquioxanes PY - 2007 SN - 0743-0515 VL - 97 SP - 444 EP - 445 PB - Division of Polymeric Materials Science and Engineering, American Chemical Society CY - Washington, DC AN - OPUS4-15846 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Frunza, L. A1 - Schönhals, Andreas A1 - Frunza, S. A1 - Parvulescu, V.I. A1 - Cojocaru, B. A1 - Carriazo, D. A1 - Martín, C. A1 - Rives, V. T1 - Rotational Fluctuations of Water Confined to Layered Oxide Materials - Nonmonotonous Temperature Dependence of Relaxation Times N2 - The rotational molecular dynamics of water confined to layered oxide materials with brucite structure was studied by dielectric spectroscopy in the frequency range from 10-2 to 107 Hz and in a broad temperature interval. The layered double hydroxide samples show one relaxation process, which was assigned to fluctuations of water molecules forming a layer, strongly adsorbed to the oxide surface. The temperature dependence of the relaxation rates has an unusual saddlelike shape characterized by a maximum. The model of Ryabov et al. (J. Phys. Chem. B 2001, 105, 1845) recently applied to describe the dynamics of water molecules in porous glasses is employed also for the layered materials. This model assumes two competing effects: rotational fluctuations of water molecules that take place simultaneously with defect formation, allowing the creation of free volume necessary for reorientation. The activation energy of rotational fluctuations, the energy of defect formation, a pre-exponential factor, and the defect concentration are obtained as main parameters from a fit of this model to the data. The values of these parameters were compared with those found for water confined to nanoporous molecular sieves, porous glasses, or bulk ice. Several correlations were discussed in detail, such as the lower the value of the energy of defect formation, the higher the number of defects. The pre-exponential factor increases with increasing activation energy, as an expression of the compensation law, and indicates the cooperative nature of the motional process. The involvement of the surface OH groups and of the oxygen atoms of the interlayer anions in the formation of hydrogen bonds was further discussed. For the birnessite sample, the relaxation processes are probably overlaid by a dominating conductivity contribution, which is analyzed in its frequency and temperature dependence. It is found that the conductivity of birnessite obeys the characteristics of semiconducting disordered materials. Especially the Barton/Nakajima/Namikawa relationship is fulfilled. Analyzing the temperature dependence of the direct current (dc) conductivity σ0 in detail gives some hint that σ0(T) has also an unusual saddlelike form. PY - 2007 DO - https://doi.org/10.1021/jp0717140 SN - 1089-5639 SN - 1520-5215 VL - 111 IS - 24 SP - 5166 EP - 5175 PB - Soc. CY - Washington, DC AN - OPUS4-15718 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Reimund, Verena A1 - Pelkner, Matthias A1 - Neubauer, Andreas A1 - Thomas, Hans-Martin A1 - Kreutzbruck, Marc T1 - Automatische Detektion von Rissen in Stahlbauteilen unter Verwendung von GMR-Sensoren bei der magnetischen Streuflussprüfung N2 - GMR-Sensor Arrays ermöglichen eine örtlich hoch aufgelöste Messung magnetischer Streufeldamplituden an Stahlbauteilen, bei der abhängig von der Größe der zu prüfenden Oberfläche erhebliche Datenmengen erzeugt werden. Eine automatische Detektion von Rissen kann anschließend mittels digitaler Bildverarbeitung erreicht werden, welche hauptsächlich auf einer Kantenerkennung basiert. Diese wurde anhand einer Magnetometer-Messung getestet, die an einem zylindersymmetrischem Bauteil mit funkenerosiv eingebrachten Rissen geringer Tiefe durchgeführt wurde. Die erzielte Selektion der Defekte wird für eine angestrebte Rekonstruktion der Defektgeometrie benötigt. T2 - DGZfP-Jahrestagung 2011 CY - Bremen, Deutschland DA - 30.05.2011 KW - GMR-Sensor KW - Streuflussprüfung PY - 2011 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-253451 SN - 978-3-940283-33-7 IS - DGZfP-BB 127 (Mo.3.C.4) SP - 1 EP - 7 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung (DGZfP) AN - OPUS4-25345 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Pelkner, Matthias A1 - Neubauer, Andreas A1 - Blome, Mark A1 - Reimund, Verena A1 - Thomas, Hans-Martin A1 - Kreutzbruck, Marc ED - Chady, T. ED - Gratkowski, S. ED - Takagi, T. ED - Udpa, S.S. T1 - Flux leakage measurements for defect characterization using NDT adapted GMR sensors N2 - High-precision magnetic field sensors are of increasing interest in non destructive testing (NDT). In particular GMR-sensors (giant magneto resistance) are qualified because of their high sensitivity, high signal-to-noise ratio and high spatial resolution. We performed magnetic flux leakage measurements of artificial cracks with a GMR-gradiometer and a 3-axes GMR-magnetometer. Cracks of a depth of 44 μm still could be detected with a sufficient high signal-to-noise ratio. A semi-analytic magnetic dipole model was used for swiftly predicting magnetic stray fields. The reliable reconstruction based on measurements of artificial rectangular-shaped defects is demonstrated. KW - GMR KW - NDT KW - Magnetic flux leakage KW - Reconstruction PY - 2011 SN - 978-1-60750-749-9 SN - 1383-7281 N1 - Serientitel: Studies in applied electromagnetics and mechanics – Series title: Studies in applied electromagnetics and mechanics VL - 35 SP - 217 EP - 224 PB - IOS Press CY - Amsterdam, The Netherlands AN - OPUS4-25374 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rosemann, P. A1 - Müller, Thoralf A1 - Babutzka, Martin A1 - Heyn, Andreas ED - J. Grosch, ED - E.J. Mittemeijer, T1 - Qualitätsbewertung von Schneidwaren durch Kurzzeit-Korrosionsprüfung N2 - Bei der Qualitätsbewertung von Schneidwaren aus nichtrostenden martensitischen Chrom-Stählen stellt die Überprüfung der Korrosionsbeständigkeit ein wichtiges Kriterium dar. Allgemein üblich sind Wechseltauchversuche mit relativ hohem zeitlichem und auswertungsbedingtem Aufwand, die noch dazu zerstörend sind und teilweise fragwürdige Ergebnisse liefern. In den letzten Jahren wurden neue Ansatze der Prüfung geschaffen, die eine nahezu zerstörungsfreie Kurzzeit-Korrosionsprüfung erlauben. Es wird gezeigt, dass mit dem elektrochemischen Rauschen sehr empfindlich Einflüsse des Härtens und der Oberflächenbehandlung auf die Korrosionsbeständigkeit nachgewiesen werden können, wodurch eine schnelle und objektive Qualitätsbewertung innerhalb des Fertigungsprozesses und der Endkontrolle von Produkten möglich ist. Das für die Prüfmethodik ausgenutzte Phänomen des elektrochemischen Rauschens zielt darauf ab, den Beginn der Korrosion empfindlich und schnell zu detektieren, ohne die Prüfbedingungen maßlos zu verschärfen und Produkte damit zu zerstören. Neben der Funktionalität der Prüfung stehen aber auch die Anwenderfreundlichkeit und somit die Akzeptanz bei den Herstellern im Vordergrund. Aus diesem Grund wurde zusätzlich ein Indikatortest (KorroPad) als praxistaugliche Alternative zum elektrochemischen Rauschen angewendet. Die Ergebnisse zeigen eine gute Übereinstimmung beider Methoden und ermöglichen eine effektive betriebliche Qualitätsüberwachung von Schneidwaren. KW - Schneidwaren KW - Nichtrostender Stahl KW - Korrosion KW - Prüfmethoden KW - Qualitätskontrolle KW - Cutlery KW - Stainless steel KW - Corrosion KW - Testing methods KW - Quality control PY - 2013 DO - https://doi.org/10.3139/105.110195 SN - 1867-2493 VL - 68 IS - 5 SP - 224 EP - 235 PB - Hanser CY - München AN - OPUS4-29341 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Hasenstab, Andreas A1 - Rieck, C. A1 - Hillemeier, B. A1 - Krause, Martin T1 - Hohlstellenortung in Holzbalken mit dem Ultraschallverfahren N2 - Zusammenfassung Die Anwendung des Ultraschallecho-Verfahrens zur Hohlstellenortung in Holzbalken wird beschrieben. An Hand der Versuchsergebnisse wird der Einfluss der Anisotropie des Holzes auf die Messkopfanordnung und Schallgeschwindigkeit dargestellt. Mit der optimierten Messanordnung ist die erfolgreiche Detektierung von Nachbildungen von Minderdicken und Kernfäule möglich. Besonders klar sind Schäden in Faserrichtung (Kernfäulenachbildung) nachzuweisen. Die sehr guten Ergebnisse zeigen die Anwendbarkeit des Ultraschallecho-Verfahrens an Holz. T2 - Jahrestagung Zerstörungsfreie Materialprüfung 2002 CY - Weimar, Deutschland DA - 2002-05-06 KW - ZfP an Holzbauteilen KW - Fehlstellen KW - Minderdicken KW - Ultraschallecho-Experimente an Probekörpern PY - 2002 UR - http://www.ndt.net/article/dgzfp02/papers/p32/p32.htm SN - 3-931381-39-0 N1 - Serientitel: Berichtsband / Deutsche Gesellschaft für zerstörungsfreie Prüfung e. V. – Series title: Berichtsband / Deutsche Gesellschaft für zerstörungsfreie Prüfung e. V. IS - 80-CD PB - DGZfP CY - Berlin AN - OPUS4-1937 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Babutzka, Martin A1 - Valet, Svenja A1 - Kotula, Stefan A1 - Burkert, Andreas A1 - Gümmer, K. A1 - Bender, S. A1 - Huckshold, M. T1 - Normentwurf für ein Prüfverfahren zur Bestimmung von Deckschichtwiderständen an Zinküberzügen mittels gelartiger Elektrolyte N2 - Das Grundproblem der heute verfügbaren und normativ geregelten Prüfverfahren für Zinküberzüge besteht neben den realitätsfernen Prüfbedingungen vor allem in der subjektiv geprägten Auswertung der Prüfergebnisse. Die systematische Betrachtung der Entwicklungen der letzten Jahre zeigt, dass die üblichen Verfahren den aktuellen Anforderungen damit schon vom Ansatz her nicht gerecht werden können und auch die bisher betriebene, fortlaufende Variation und Anpassung von Prüfbedingungen keinen grundlegend neuen Lösungsansatz bieten können. Ein solcher ergibt sich nur, wenn die Zinküberzüge hinsichtlich der kinetischen Eigenschaften der Deckschichtbildung und -auflösung umfassend beschrieben werden können, was nur durch den Einsatz elektrochemischer Untersuchungsmethoden mittels Gelelektrolyten möglich ist. Aus diesem Grund wurde im Verbundforschungsvorhaben GELELEK auf der Basis elektrochemischer Methoden unter Verwendung eines Gelelektrolyten ein Normenvorschlag für eine Prüfnorm erarbeitet und zur Normungsreife geführt, welcher den Anforderungen an ein Messsystem für Feldanwendungen entspricht. Im Verbundforschungsvorhaben GELELEK wurde eine gezielte Kombination von Laboruntersuchungen mit Untersuchungen im Feld und Bauteilen unter realen Einsatzbedingungen angestrebt. Randbedingungen für eine gesicherte Messung von atmosphärisch bewitterten Zinküberzügen unter Einsatz von Gelelektrolyten wurden erarbeitet und im Normenvorschlag festgeschrieben. Darüber hinaus wurde ein mobiles Messgerät für Messungen mit Gelelektrolyten an realen Bauteilen entwickelt. Nach Abschluss des Forschungsvorhabens steht Industrievertretern und Prüfinstituten ein wissenschaftlich gesichertes Messverfahren basierend auf Kennwerten zur Verfügung, um Zinküberzüge und deren momentane Schutzwirkung unter praxisrelevanten Bedingungen einschätzen und normativ geregelt prüfen zu können. Der vorliegende Forschungsbericht gibt einen Überblick über die Motivation zur Durchführung des Forschungsvorhabens, wichtige Arbeitsschritte, Details zur entwickelten Prüfmethode sowie Einsatzmöglichkeiten für Prüfinstitute und Unternehmen. KW - Normung KW - Zink KW - Korrosion KW - Deckschichtbildung KW - Atmosphärische Korrosion KW - Korrosionsprüfung PY - 2022 UR - https://www.gav-verzinken.de/forschung/wissenspool SP - 1 EP - 24 AN - OPUS4-54947 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Szymoniak, Paulina A1 - Kolmangadi, Mohamed A. A1 - Böhning, Martin A1 - Frick, B. A1 - Apple, M. A1 - Mole, R. A. A1 - De Souza, N. R. A1 - Zorn, R. A1 - Schönhals, Andreas T1 - Confined Segmental Diffusion in Nanophase Separated Janus Polynorbornenes as Investigated by Quasielastic Neutron Scattering N2 - A combination of neutron time-of-flight and neutron backscattering spectroscopy was used to investigate the molecular dynamics of Janus polynorbornenes (Janus poly(tricyclononenes)) on a microscopic level. These Janus polynorbornenes, denoted as PTCNSiOR, have a semirigid backbone with −Si(OR)3 side groups attached to it. R represents the length of the alkyl side chain. Here side chain lengths of R = 3 (propyl) and R = 8 (octyl) were considered. It is worth mentioning that these polymers have some potential as active layers in gas separation membranes, especially for the separation of higher hydrocarbons. The combination of time-of-flight and backscattering will ensure a reasonably broad time window for analysis where the incoherent intermediate scattering function SInc(q,t) is considered. Previously, it was shown by X-ray investigations that the system undergoes a nanophase separation into alkyl side chain-rich domains surrounded by a backbone-rich matrix. For PTCNSiOPr (R = 3), the alkyl side-chain-rich domains are truly isolated in the backbone-rich matrix, whereas for PTCNSiOOc (R = 8) these domains percolate through the matrix. Further, it was also previously shown that the alkyl side-chain-rich domains undergo a glass transition. The advantage of neutron scattering experiments discussed here is that besides temporal also spatial information is obtained which will allow conclusions to be drawn about the type of molecular fluctuations. At the lowest measured temperature, the decay in Sinc(q,t) is due to the methyl group rotation. The methyl group dynamics is analyzed in terms of a modified jump-diffusion in a 3-fold potential and yields to a reasonable fraction of hydrogens which contribute to the methyl group rotation. At higher temperatures, the decay in SInc(q,t) is due to both the methyl group rotation and the segmental dynamics in the alkyl side-chain-rich domains. The segmental diffusion is modeled by a sublinear diffusion. For the analysis of the scattering function SInc(q,t) of PTCNSiOPr an elastic scattering due to the immobilized backbone-rich matrix must be taken into account. The analysis reveals that the segmental dynamics is confined by the finite size of alkyl chain-rich domains and that it is intrinsically heterogeneous in nature. Both effects are more pronounced for PTCNSiOPr in comparison to those of PTCNSiOOc. KW - Polynorbornene KW - Quasielastic Neutron Scattering PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-608712 DO - https://doi.org/10.1021/acs.macromol.4c01045 SP - 1 EP - 14 PB - ACS Publications AN - OPUS4-60871 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Szymoniak, Paulina A1 - Kolmangadi, Mohamed A. A1 - Böhning, Martin A1 - De Souza, N. R. A1 - Juranyi, F. A1 - Zorn, R. A1 - Schönhals, Andreas T1 - Inelastic and Quasielastic Neutron Scattering on Polynorbornenes with Bulky Carbocyclic Side groups N2 - This study investigates the molecular mobility and vibrational properties of polynorbornenes with bulky carbocyclic side groups using inelastic and quasielastic neutron scattering techniques. The polymers, synthesized via metathesis and addition polymerization, exhibit varying degrees of microporosity, which ignificantly influences their gas separation performance. By inelastic neutron scattering experiments, it could be shown that all considered polymers have excess contributions to the low frequency vibrational density of states known as the Boson peak. The maximum frequency of the Boson peak correlates to the microporosity of the polymers. This correlation supports the sound wave interpretation of the Boson peak, suggesting that the microporous structure enhances the compressibility of the material at a microscopic length scale. The molecular mobility, particularly the methyl group rotation, was characterized using elastic scans and quasielastic neutron scattering. The study revealed a temperature dependent relaxation process, with the onset of molecular fluctuations observed around 200 K for the polymer containing methyl groups. For the polymer having no methyl groups only elastic scattering is observed. The methyl group rotation was analyzed in terms of a jump diffusion in a threefold potential with three equivalent energy minima. This leads to an almost correct description of the q dependence of the elastic incoherent scattering function when the number of hydrogen nuclei undergoing the methyl group rotation is considered. It was further evidenced that the fraction of methyl undergoing the methyl group rotation increases with increasing temperature. KW - Polymers of Intrinsic Microporosity KW - Neutron scattering PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-630297 DO - https://doi.org/10.1016/j.polymer.2025.128358 SN - 1873-2291 VL - 328 SP - 241 PB - Elsevier Ltd. AN - OPUS4-63029 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zorn, R. A1 - Szymoniak, Paulina A1 - Kolmangadi, Mohamed Aejaz A1 - Malpass-Evans, R. A1 - McKeown, N. A1 - Jalarvo, N. A1 - Tyagi, M. A1 - Böhning, Martin A1 - Schönhals, Andreas T1 - Microscopic molecular mobility of high-performance polymers of intrinsic microporosity revealed by neutron scattering – bend fluctuations and signature of methyl group rotation N2 - Polymers of intrinsic microporosity exhibit a combination of high gas permeability and reasonable permselectivity, which makes them attractive candidates for gas separation membrane materials. The diffusional selective gas transport properties are connected to the molecular mobility of these polymers in the condensed state. Incoherent quasielastic neutron scattering was carried out on two polymers of intrinsic microporosity, PIM-EA-TB(CH3) and its demethylated counterpart PIM-EA-TB(H2), which have high Brunauer–Emmett–Teller surface area values of 1030 m2 g-1 and 836 m2 g-1, respectively. As these two polymers only differ in the presence of two methyl groups at the ethanoanthracene unit, the effect of methyl group rotation can be investigated solely. To cover a broad dynamic range, neutron time-of-flight was combined with neutron backscattering. The demethylated PIM-EA-TB(H2) exhibits a relaxation process with a weak intensity at short times. As the backbone is rigid and stiff this process was assigned to bendand-flex fluctuations. This process was also observed for the PIM-EA-TB(CH3). A further relaxation process is found for PIM-EA-TB(CH3), which is the methyl group rotation. It was analyzed by a jump-diffusion in a three-fold potential considering also the fact that only a fraction of the present hydrogens in PIM-EATB(CH3) participate in the methyl group rotation. This analysis can quantitatively describe the q dependence of the elastic incoherent structure factor. Furthermore, a relaxation time for the methyl group rotation can be extracted. A high activation energy of 35 kJ mol-1 was deduced. This high activation energy evidences a strong hindrance of the methyl group rotation in the bridged PIM-EA-TB(CH3) structure. KW - Polymers of Intrinsic Microporosity KW - Neutron Scattering PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-604114 DO - https://doi.org/10.1039/d4sm00520a SP - 1 EP - 11 PB - RSC AN - OPUS4-60411 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zorn, R. A1 - Szymoniak, Paulina A1 - Kolmangadi, Mohamed Aejaz A1 - Malpass-Evans, R. A1 - McKeown, N. A1 - Tyagi, M. A1 - Böhning, Martin A1 - Schönhals, Andreas T1 - Low frequency vibrations and diffusion in disordered polymers bearing an intrinsic microporosity as revealed by neutron scattering N2 - The microscopic diffusion and the low frequency density of states (VDOS) of PIM-EATB(CH3) are investigated by inelastic and quasi-elastic neutron scattering where also the demethylated counterpart of PIM-EA-TB(H2) is considered. These intrinsic microporous polymers are characterized by large BET surface area values of several hundred m2/g and pore sizes between 0.5 and 2 nm. Detailed comparison is made to the archetype of polymers of intrinsic microporosity, PIM-1, and polynorbornenes also bearing a microporosity. Due to the wavelength of neutrons, the diffusion and vibrations can be addressed on microscopic length and time scales. From the inelastic neutron scattering experiments the low frequency density of states (VDOS) is estimated which shows excess contributions to the Debye-type VDOS known as Boson peak. It was found that the maximum frequency of the Boson peak decreases with increasing microporosity characterized by the BET surface area. However, besides the BET surface area, additional factors such as the backbone stiffness govern the maximum frequency of the Boson peak. Further the mean squared displacement related to microscopic motions was estimated from elastic fixed window scans. At temperatures above 175 K, the mean squared displacement PIM-EA-TB(CH3) is higher than that for the demethylated counterpart PIM-EA-TB(H2). The additional contribution found for PIM-EATB(CH3) is ascribed to the rotation of the methyl group in this polymer because the only difference between the two structures is that PIM-EA-TB(CH3) has methyl groups where PIM-EA-TB(H2) has none. A detailed comparison of the molecular dynamics is also made to that of PIM-1 and the microporous polynorbornene PTCNSi1. The manuscript focuses on the importance of vibrations and the localized molecular mobility characterized by the microscopic diffusion on the gas Transport in polymeric separation membranes. In the frame of the random gate model localized fluctuations can open or close bottlenecks between pores to enable the diffusion of gas molecules. KW - Polymer of intrisic microporosity KW - Neutron scattering KW - Boson peak KW - Methyl group rotation PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-538490 DO - https://doi.org/10.3390/cryst11121482 VL - 11 IS - 12 SP - 1 EP - 16 PB - MDPI CY - Basel AN - OPUS4-53849 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kolmangadi, Mohamed Aejaz A1 - Szymoniak, Paulina A1 - Zorn, R. A1 - Böhning, Martin A1 - Wolff, M. A1 - Zamponi, M. A1 - Schönhals, Andreas T1 - Molecular mobility in high-performance polynorbornenes:A combined broadband dielectric, advanced calorimetry,and neutron scattering investigation N2 - The molecular dynamics of two addition type polynorbornenes, exo-PNBSiand PTCNSi1, bearing microporosity has been investigated by broadbanddielectric spectroscopy, fast scanning calorimetry, and neutron scattering. Bothpolymers have the same side groups but different backbones. Due to theirfavorable transport properties, these polymers have potential applications inseparation membranes for gases. It is established in literature that molecularfluctuations are important for the diffusion of small molecules through poly-mers. For exo-PNBSi, two dielectric processes are observed, which are assignedto Maxwell/Wagner/Sillars (MWS) process due to blocking of charge carriersat internal voids or pore walls. For PTCNSi1, one MWS-polarization process isfound. This points to a bimodal pore-size distribution for exo-PNBSi. A glasstransition for exo-PNBSi and for PTCNSi1 could be evidenced for the first timeusing fast scanning calorimetry. For Tgand the corresponding apparent activa-tion energy, higher values were found for PTCNSi1 compared to exo-PNBSi.For both polymers, the neutron scattering data reveal one relaxation process.This process is mainly assigned to methyl group rotation probably overlayedby carbon–carbon torsional fluctuations. KW - Advanced calorimetry KW - Dielectric spectroscopy KW - Neutron scattering KW - Polynorbornenes PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-547086 DO - https://doi.org/10.1002/pen.25995 SN - 0032-3888 VL - 62 IS - 7 SP - 2143 EP - 2155 PB - Wiley AN - OPUS4-54708 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -