TY - JOUR A1 - Gaal, Mate A1 - Bovtun, Viktor A1 - Stark, Wolfgang A1 - Erhard, Anton A1 - Yakymenko, Y. A1 - Kreutzbruck, Marc T1 - Viscoelastic properties of cellular polypropylene ferroelectrets N2 - Viscoelastic properties of cellular polypropylene ferroelectrets (PP FEs) were studied at low frequencies (0.3–33 Hz) by dynamic mechanical analysis and at high frequencies (250 kHz) by laser Doppler vibrometry. Relaxation behavior of the in-plane Young’s modulus (Y´ 11~1500 MPa at room temperature) was observed and attributed to the viscoelastic response of polypropylene matrix. The out-of-plane Young’s modulus is very small (Y´33≈0.1 MPa) at low frequencies, frequency- and stress-dependent, evidencing nonlinear viscoelastic response of PP FEs. The highfrequency mechanical response of PP FEs is shown to be linear viscoelastic with Y´33≈0.8 MPa. It is described by thickness vibration mode and modeled as a damped harmonic oscillator with one degree of freedom. Frequency dependence of Y*33 in the large dynamic strain regime is described by the broad Cole-Cole relaxation with a mean frequency in kHz range attributed to the Dynamics of the air flow between partially closed air-filled voids in PP FEs. Switching-off the relaxation contribution causes dynamic crossover from the nonlinear viscoelastic regime at low frequencies to the linear viscoelastic regime at high frequencies. In the small strain regime, contribution of the air flow seems to be insignificant and the power-law response, attributed to the mechanics of polypropylene cell walls and closed air voids, dominates in a broad frequency range. Mechanical Relaxation caused by the air flow mechanism takes place in the sound and ultrasound frequency range (10 Hz–1MHz) and, therefore, should be taken into account in ultrasonic applications of the PP FEs deal with strong exciting or receiving signals. KW - Viscoelastic KW - Cellular polypropylene KW - Ferroelectret PY - 2016 U6 - https://doi.org/10.1063/1.4944798 SN - 0021-8979 SN - 1089-7550 SN - 1520-8850 VL - 119 SP - Article Number: 125101 PB - AIP Publishing AN - OPUS4-35956 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - McHugh, Jarlath A1 - Stark, Wolfgang T1 - Determination and interpretation of changes in thermophysical properties of a carbon-fibre prepreg during cure N2 - Epoxy composites used for high-end structural applications are typically cured under the influence of temperature and pressure causing a number of complex chemical and physical transformations. On heating a mould, temperature gradients will occur through the component which will depend largely on the thermophysical properties of the specific composite. The crosslinking reaction is exothermic leading to additional heat release, thus complicating heat transportation models. If such effects are not accounted for, it can lead to variations in resin flow, poor fibre wetting causing voiding and inhomogeneous cure, leading to shrinkage and unfavourable variations in moulded part geometry. Limited information is available for thermal models used in the manufacture of reinforced thermosets. Autoclave [1, 2] and laser or infra-red curing processes [3, 4] typically use constant values determined on fully cured parts. In this work, the variation in thermal conductivity (K) (W/(m K)), thermal diffusivity (a) (m(2)/s) and specific heat capacity at constant pressure (c(p)) (J/(g K) is determined for a carbon fibre prepreg during cure. It is the intention to improve understanding of how these parameters are related to chemical or physical transformations occurring during cure, and where estimates or shortcuts may be used for heat transfer models KW - Differential scanning calorimetry KW - Temerature KW - Epoxy system PY - 2016 U6 - https://doi.org/10.1016/j.polymertesting.2015.11.015 SN - 0142-9418 VL - 49 SP - 115 EP - 120 PB - Elsevier Science CY - Oxford AN - OPUS4-35788 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stark, Wolfgang A1 - Jaunich, Matthias A1 - Mc Hugh, Jarlath T1 - Dynamic mechanical analysis (DMA) of epoxy carbon-fibre prepregs partially cured in a discontinued autoclave analogue process N2 - Epoxy carbon-fibre prepreg, Hexcel Type 6376 HTS, was investigated using Dynamic Mechanical Analysis (DMA). The DMA characteristic parameters are storage modulus E', loss modulus E' and loss factor tanδ. These parameters are ideally suited to observe the vitrification, referred to as glass transition, resulting from the cross-linking reaction. Detection of the cure state may also be achieved by determining the momentary glass transition temperature of partially cured samples. The consequent use of a multi-frequency measuring regime was used to derive the apparent activation energy for the glass transition process. Different temperature programs were also applied to monitor the curing process directly, as well as to investigate the different states of incomplete cure reached in preceding curing steps. The intention was to provide better understanding of the consequences of an interrupted autoclave curing process and to use DMA to detect the cure state achieved. With DMA, the continuation of an incomplete curing process also can be monitored. DMA measurements up to 300 °C showed, furthermore, that the final glass transition temperature was reduced by thermal degradation at high temperatures. KW - Composites KW - Epoxy KW - Cross-linking KW - Prepreg KW - Degree of cure KW - Glass transition PY - 2015 U6 - https://doi.org/10.1016/j.polymertesting.2014.11.004 SN - 0142-9418 VL - 41 SP - 140 EP - 148 PB - Elsevier Science CY - Amsterdam [u.a.] AN - OPUS4-32325 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Böhning, Martin A1 - Niebergall, Ute A1 - Adam, Adeline A1 - Stark, Wolfgang T1 - Impact of biodiesel sorption on mechanical properties of polyethylene N2 - The time-dependent sorption of biodiesel in a typical polyethylene for container applications is investigated in comparison to conventional diesel fuel at three different temperatures. In this context, the desorption behavior is also addressed. Subsequently, the effects of both penetrants on mechanical properties are characterized in terms of impact strength and dynamic-mechanical analysis. The discussion of property changes is firstly based on the sorption kinetics of biodiesel and diesel, which is determined by immersion experiments allowing for the calculation of respective diffusion coefficients. Changes in impact strength as determined by the Charpy method are further characterised in more detail by analyzing the fracture surfaces, and correlated with results of dynamic-mechanical analysis. KW - Biodiesel KW - Fuel sorption KW - Desorption KW - Impact strength KW - Dynamic-mechanical analysis KW - PE-HD PY - 2014 U6 - https://doi.org/10.1016/j.polymertesting.2013.12.003 SN - 0142-9418 VL - 34 SP - 17 EP - 24 PB - Elsevier Science CY - Amsterdam [u.a.] AN - OPUS4-30096 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gaal, Mate A1 - Bovtun, V. A1 - Stark, Wolfgang A1 - Kreutzbruck, Marc ED - Kollmeier, B. T1 - Bestimmung der elastischen Eigenschaften des Polypropylen-Ferroelektrets N2 - Ferroelektrete sind zelluläre polarisierte Polymere, die ferroelektrische und dadurch auch piezoelektrische Eigenschaften aufweisen. Unter anderem werden sie für den Bau von Mikrofonen und Ultraschallwandlern für Materialprüfung eingesetzt. Dabei erweist sich ihre besonders niedrige akustische Impedanz als Vorteil. Ursache dafür ist vor allem ihr außergewöhnlich niedriger Elastizitätsmodul in Dickenrichtung. In diesem Beitrag werden zwei Methoden für die Ermittlung des Elastizitätsmoduls des geladenen zellulären Polypropylens (zPP) dargestellt. Die erste ist eine neuartige modellgestützte Methode mittels Laservibrometrie an dem eigenentwickelten Polypropylen-Wandler, wobei die Resonanzschwingung des Wandlers bei 250 kHz gemessen wird. Die zweite Methode ist dynamisch-mechanische Analyse (DMA) durchgeführt mit Frequenzen von 0,3 bis 50 Hz, erstmalig für das zPP angewendet. T2 - DAGA 2014 - 40. Jahrestagung für Akustik CY - Oldenburg, Germany DA - 10.03.2014 PY - 2014 SN - 978-3-939296-06-5 SP - 1 EP - 2 AN - OPUS4-31368 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stark, Wolfgang A1 - Böhning, Martin A1 - Jaunich, Matthias A1 - Teteris, Gundars A1 - McHugh, J. T1 - Charakterisierung des Härtungsporozesse und Härtungszustands von Kohlefaser-Composite-Bauteilen - Thermoanalytische Labormethoden und Online-Prozesskontrolle T2 - Thermische Analyse für Polymeranwendungen CY - Berlin, Germany DA - 2014-01-22 PY - 2014 AN - OPUS4-30683 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Braun, Ulrike A1 - Brademann-Jock, Kerstin A1 - Stark, Wolfgang T1 - Cure monitoring of epoxy films by heatable in situ FTIR analysis: Correlation to composite parts N2 - The curing mechanism of an epoxy film containing dicyandiamide (DICY) and an epoxy formulation based on diglycidyl ether of Bisphenol A (DGEBA) polymer was studied as a function of various temperature programs. The investigation was performed in situ, using a thin film of the epoxy mixture on a silicon wafer substrate in a heatable transmission tool of a FTIR spectrometer. Based on these model-curing experiments, a major curing mechanism was proposed, taking into account the appearance, the decrease, and the development of characteristic bands at various temperatures. The conclusions of the model curing were correlated to FTIR measurements on a real, 50-mm-thick glass fiber reinforced component composite part from a technical process. It could be shown that characteristic bands that develop at curing temperatures above 150°C appear especially in the center of the thick sample. From the chemical or molecular point of view, this demonstrates the established technician's understanding that temperature control inside a large-scale fiber composite of, for example, aircraft, wind-turbine, automotive applications component is of major importance. KW - Crosslinking KW - Resins KW - Spectroscopy KW - Thermosets KW - Thermal properties PY - 2014 U6 - https://doi.org/10.1002/APP.39832 SN - 0021-8995 SN - 1097-4628 VL - 131 IS - 3 SP - 39832, 1 EP - 10 PB - Wiley InterScience CY - Hoboken, NJ AN - OPUS4-30716 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jaunich, Matthias A1 - Stark, Wolfgang A1 - Wolff, Dietmar T1 - Druckverformungsrest bei tiefen Temperaturen N2 - Der Druckverformungsrest (DVR) stellt insbesondere für Dichtungsanwendungen eine wichtige Kenngröße zur Beurteilung der Eignung eines Elastomers dar. Er ermöglicht die Einschätzung des zeitabhängigen Rückstellverhaltens eines Werkstoffs nach Deformation. Neben der Prüfung bei erhöhten Temperaturen, zur Beurteilung des Alterungsverhaltens, lässt sich bei der Durchführung bei tiefen Temperaturen die limitierende Einsatztemperatur bestimmen. Die Versuchsdurchführung unterscheidet sich je nach angewandter Norm und kann einen deutlichen Einfluss auf den DVR-Wert haben. Um bei tiefen Temperaturen eine schnelle Aussage zu gestatten, ist eine im Vergleich zu genormten Methoden deutlich schneller durchzuführende, automatisierte Methode entwickelt und mit Standardmethoden verglichen worden. Durch kontinuierliche Messung des Druckverformungsrests kann die Kinetik der Materialrückstellung betrachtet und dadurch ein effizienter Materialvergleich und eine effiziente Materialauswahl ermöglicht werden. Compression set (CS) is especially for sealing applications an important parameter for material selection. It allows an assessment of the time dependent recovery after deformation. In addition to testing at elevated temperatures which aims at the evaluation of the ageing behaviour, testing at low temperatures permits the determination of the low working temperature limit. The test procedure varies depending on the applied standard and can show a significant effect on the CS value. In order to allow a quick statement regarding low temperatures an automated procedure being significantly faster realisable in relation to the standardised methods has been developed and compared with standard procedures. Continuous measurement of the compression set allows evaluating the recovery kinetics and therefore an efficient comparison and selection of materials. KW - Druckverformungsrest KW - Elastomere KW - Dichtung KW - O-Ring PY - 2014 SN - 0176-1625 VL - 67 IS - 8 SP - 487 EP - 491 PB - Gupta CY - Ratingen AN - OPUS4-31572 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Böhning, Martin A1 - Niebergall, Ute A1 - Adam, Adeline A1 - Stark, Wolfgang T1 - Influence of biodiesel sorption on temperature-dependent impact properties of polyethylene N2 - In a previous paper we investigated the influence of sorbed biodiesel or diesel on mechanical properties of a typical polyethylene grade for tank applications. Besides the basic sorption and desorption behavior of these two fuels, the study addressed the concentration-dependent mechanical properties as revealed by a non-instrumented Charpy impact test and dynamic mechanical analysis (DMA). In the present paper we extend this investigation focusing on the temperature-dependent impact fracture behavior. Therefore, an instrumented Charpy impact test was employed, allowing a more detailed analysis of the fracture behavior. Furthermore, from the load-time-diagrams obtained from the instrumented impact test, corresponding fracture times can be calculated, allowing a clear correlation of the fuel sorption induced changes in fracture toughness with the enhanced ß-relaxation observed by DMA. As in the previous study, the fracture surfaces of the impact tested specimens were analyzed in order to confirm the brittle or ductile character of the fracture indicated by impact strength and the corresponding load-deflection diagrams. KW - Biodiesel KW - Fuel sorption KW - Impact strength KW - Charpy impact test KW - Dynamic-mechanical analysis KW - Relaxation KW - PE-HD PY - 2014 U6 - https://doi.org/10.1016/j.polymertesting.2014.09.001 SN - 0142-9418 VL - 40 SP - 133 EP - 142 PB - Elsevier Science CY - Amsterdam [u.a.] AN - OPUS4-31583 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wolff, Dietmar A1 - Jaunich, Matthias A1 - Stark, Wolfgang T1 - Investigating the performance of rubber seals at low temperatures N2 - Rubbers are widely used as main sealing materials for Containers for low and intermediate level radioactive waste and as additional component to metal seals in spent fuel and high active waste containers. The save enclosure of the radioactive container inventory has to be guaranteed according to legislation and appropriate guidelines for long term storage periods as well as down to temperatures of -40 °C for transportation. Therefore the understanding of failure mechanisms that lead to leakage at low temperatures is necessary to ensure a proper material choice which is certainly also influenced by additional factors as e.g. the aging behavior. T2 - 14th International high-level radioactive waste management conference CY - Albuquerque, New Mexico, USA DA - 28.04.2013 KW - Rubber seals KW - Elastomers KW - Compression set KW - Low temperature KW - Leakage rate PY - 2013 SN - 978-1-62748-644-6 SP - 1 EP - 7(Paper # 6888) PB - Omnipress AN - OPUS4-28530 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -