TY - JOUR A1 - Buchholz, Uwe A1 - Jaunich, Matthias A1 - Stark, Wolfgang A1 - Habel, Wolfgang A1 - Petersson, B.A.T. T1 - Acoustic data of cross linked polyethylene (XLPE) and cured liquid silicone rubber (LSR) by means of ultrasonic and low frequency DMTA N2 - Partial discharges may cause damage to electrical insulation of high voltage equipment. They initiate elastic waves in the insulating material, e.g. in the stress cone of an outdoor termination. Localisation of the origin of such elastic waves can help to predict serious damaging processes in the electrical insulation. In order to measure and evaluate the wave propagation effects in typical multilayered elastomeric structures, knowledge of the material properties is required. The propagating velocity and the attenuation of longitudinal waves are important parameters. Values for these quantities found in the literature were not appropriate. Therefore, for cross-linked polyethylene (XLPE) and cured liquid silicone rubber (LSR), the longitudinal wave velocity and the attenuation were evaluated in the temperature interval from -20°C to 50°C and in the frequency range from 200 kHz to 600 kHz using a two-sample ultrasound technique. The loss factor was determined from these measured quantities. Additionally, low frequency Dynamic Mechanical Thermal Analysis (DMTA) was applied to investigate LSR and XLPE in a temperature interval between -100 and 50°C and to check qualitatively the ultrasound data. KW - Acoustic propagation KW - Cross linked polyethylene insulation KW - Mechanical variables measurement KW - Silicone rubber PY - 2012 DO - https://doi.org/10.1109/TDEI.2012.6180250 SN - 1070-9878 SN - 0018-9367 SN - 1558-4135 VL - 19 IS - 2 SP - 558 EP - 566 PB - Institute of Electrical and Electronics Engineers CY - New York, NY AN - OPUS4-26106 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 DO - 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 - 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 DO - 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 - 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 DO - 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 - 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 DO - 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 - Bartusch, Jürgen A1 - Döring, Joachim A1 - Mc Hugh, Jarlath T1 - Making cure visible: monitoring the crosslinking process using integrated ultrasound sensors N2 - A special ultrasonic measuring system was developed to monitor the cross-linking process, enabling interaction with the manufacturing process in order to optimise part quality and reduce cycle times. KW - Thermoset KW - Ultrasound sensors KW - Mould KW - Rtm KW - Gelation KW - Vitrification PY - 2008 SN - 1639-965X IS - 38 SP - 64 EP - 66 PB - JEC CY - Paris AN - OPUS4-18610 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stark, Wolfgang A1 - Goering, Harald A1 - Michel, U. A1 - Bayerl, H. T1 - Online monitoring of thermoset post-curing by dynamic mechanical thermal analysis DMTA N2 - Thermosetting moulding compounds are synthetic materials which can be easily formed in the molten state and achieve high temperature stability due to a cross-linking process which takes place during manufacture. To ensure thermal and mechanical properties, post-curing of moulded phenolic resin components is necessary for high quality applications. In the industrial practice, post-curing time-temperature-programs are heuristically acquired. In this paper, dynamical mechanical thermal analysis is employed to determine optimal post-curing conditions for injection moulded parts from phenolic resin. KW - DMTA KW - Moulding compound KW - Thermoset KW - Phenolic resin KW - Post-curing PY - 2009 DO - https://doi.org/10.1016/j.polymertesting.2009.02.005 SN - 0142-9418 VL - 28 IS - 6 SP - 561 EP - 566 PB - Elsevier Science CY - Amsterdam [u.a.] AN - OPUS4-19822 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stark, Wolfgang T1 - Development of quality assurance for insulating materials PY - 2010 UR - https://www.google.de/url?sa=t&rct=j&q=&esrc=s&source=web&cd=1&ved=0ahUKEwjyyejZ7tvKAhXBVxoKHeV0Dr4QFgghMAA&url=https%3A%2F%2Fwww.kunststoffe.de%2Fen%2F_storage%2Fasset%2F590842%2Fstorage%2Fmaster%2Ffile%2F6128237%2Fdownload%2FDevelopment%2520of%2520Quality%2520Assurance%2520for%2520Insulating%2520Materials.pdf&usg=AFQjCNGMbKTaYDrHEdGuZ2IB_7zQCrTVkw SN - 1862-4243 VL - 100 IS - 2 SP - 6 EP - 9 PB - Hanser CY - München AN - OPUS4-20936 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stark, Wolfgang T1 - Investigation of curing behaviour of melamine/phenolic (MP) thermosets N2 - Commercially available melamine/phenolic (MP) moulding compounds used for manufacturing electro installation parts were investigated by laboratory thermal analysis methods: Dynamic Mechanical Analysis (DMA), Differential Scanning Calorimetry (DSC) and Dielectric Analysis (DEA). The results were compared with on-line measurements in a compression mould using incorporated dielectric and ultrasound sensors. Softening and cross-linking behaviour were analyzed. For on-line process monitoring, only the ultrasound method worked well. The dielectric method was distorted by water formed as a by-product from the poly-condensation reaction. KW - Thermoset KW - Melamine KW - Phenol KW - Moulding compound KW - Cross-linking KW - DSC PY - 2010 DO - https://doi.org/10.1016/j.polymertesting.2010.05.008 SN - 0142-9418 VL - 29 IS - 6 SP - 723 EP - 728 PB - Elsevier Science CY - Amsterdam [u.a.] AN - OPUS4-20982 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mc Hugh, Jarlath A1 - Fideu, P. A1 - Herrmann, A. A1 - Stark, Wolfgang T1 - Determination and review of specific heat capacity measurements during isothermal cure of an epoxy using TM-DSC and standard DSC techniques N2 - The technique normally used to measure Cp during isothermal cure is Temperature Modulated - Dynamic Scanning Calorimetry TM-DSC. It is however not standardised, experimentally complicated and quite time intensive. As will be shown, Cp may also be estimated during isothermal cure just from using dynamic heating experiments on a fully cured sample. Such values are often sufficient for isothermal heat transfer models that otherwise employ a constant Cp value obtained from the fully cured epoxy. Secondly, the results from dynamic heating experiments provide a quick means, in comparison to isothermal TMDSC measurements, of estimating Cp variation during cure as well as providing a good estimate value for Cp towards the end of isothermal cure. As will be shown, such values obtained from a standardised measurement procedure are very helpful in setting up TMDSC experiments that are more sensitive to experimental error influenced by factors such as sample weight and geometry. The DSC results illustrate that the measured heat capacity Cp for a fully cured epoxy over a temperature range are very similar to values for samples partially cured at corresponding isothermal temperatures, under the prerequisite that vitrification takes place. In such cases the primary influence on Cp is specific measurement temperature and not degree of cure. For isothermal cure temperatures investigated between 150 and 200 °C, the total change of Cp during cure is nearly constant and correlates well with values published by authors on other epoxy based systems. Taking Cp variation as constant, it is possible from just dynamic heating experiments on the cured epoxy to estimate Cp for the uncured epoxy system at specific cure temperatures. The next step would be to estimate the full Cp profile during isothermal cure, however, in such cases, the time to vitrification would also be needed as additional information. PY - 2010 DO - https://doi.org/10.1016/j.polymertesting.2010.04.004 SN - 0142-9418 VL - 29 IS - 6 SP - 759 EP - 765 PB - Elsevier Science CY - Amsterdam [u.a.] AN - OPUS4-21916 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -