TY - JOUR A1 - Bovtun, V. A1 - Stark, Wolfgang A1 - Kelm, Jürgen A1 - Porokhonskyy, V. A1 - Yakimenko, Y. T1 - Microwave Dielectric Properties of Rubber Compounds Undergoing Vulcanisation - Part 2. Influence of Carbon Black N2 - The application of microwave measurements to the characterisation of rubber compounds vulcanisation is considered. The behaviour of mechanical and microwave (20 GHz) dielectric parameters during vulcanisation was investigated for rubber compounds with different concentrations of active and non-active carbon black. An increase of concentration or activity of carbon black results in the increase of both dielectric permittivity ε?(T) and loss ε?(T) and in the increase of torsion modulus as well. The start of the vulcanisation reaction is indicated by an increase of dielectric permittivity and torsion modulus in all investigated unvulcanised compounds with carbon black. While for compounds with non-active carbon black the vulcanisation can be better indicated by the ε?(T) anomaly, for compounds with active carbon black it is more clearly seen by the change of ε?(T) behaviour. PY - 2002 UR - http://www.plastverarbeiter.de/ai/resources/d5af83c1e48.pdf SN - 0948-3276 SN - 0022-9520 VL - 55 IS - 1-2 SP - 16 EP - 22 PB - Hüthig CY - Heidelberg AN - OPUS4-1564 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bovtun, V. A1 - Stark, Wolfgang A1 - Pashkov, V. A1 - Kelm, Jürgen A1 - Yakimenko, Y. T1 - Microwave On-Line Monitoring of Thermoset Curing PY - 2002 SN - 0025-5300 VL - 44 IS - 7-8 SP - 300 EP - 306 PB - Carl Hanser Verlag CY - München AN - OPUS4-1563 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bovtun, Viktor Petrovic A1 - Stark, Wolfgang A1 - Kelm, Jürgen A1 - Pashkov, V.M. A1 - Yakimenko, Y. T1 - Characterization of carbon black filled rubber compounds by the Microwave Coaxial Method KW - Dielectric parameters KW - Microwave methods KW - Filled rubber compounds KW - Vulcanisation PY - 2005 SN - 0025-5300 VL - 47 IS - 3 SP - 118 EP - 122 PB - Carl Hanser Verlag CY - München AN - OPUS4-7273 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bovtun, Viktor Petrovic A1 - Stark, Wolfgang A1 - Kelm, Jürgen A1 - Porokhonskyy, V. A1 - Yakimenko, Y. T1 - Microwave Dielectric Properties of Rubber Compounds Undergoing Vulcanisation - Part 1. Natural rubber with and without carbon black filler KW - Dielectric parameters KW - Microwave methods KW - Vulcanisation KW - Elastomers KW - Monitoring PY - 2000 SN - 0948-3276 SN - 0022-9520 PB - Hüthig CY - Heidelberg AN - OPUS4-1062 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 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 - 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 U6 - 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 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 - 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 - JOUR A1 - Cappella, Brunero A1 - Stark, Wolfgang T1 - Adhesion of amorphous polymers as a function of temperature probed with AFM force-distance curves N2 - Force–displacement curves have been obtained with a commercial atomic force microscope at different temperatures and probe rates on a thick film of poly(n-butyl methacrylate) and on two films of polystyrene with different molecular weight. In a previous publication [B. Cappella, S.K. Kaliappan, H. Sturm, Macromolecules 38 (2005)1874] the analysis of force–displacement curves has been focused on the stiffness and on the Young's modulus of the samples. In the present publication we consider the temperature dependence of the work of adhesion. We have obtained master curves of the work of adhesion at fixed maximum loads and, by comparing the results of the two analysis, we show that the work of adhesion follows the Williams–Landel–Ferry equation with the same coefficients previously found for the Young's modulus. Furthermore, we show that the temperature dependence of the work of adhesion of the polymers is a consequence of the temperature dependence of the tip–sample contact area and in the end of the temperature dependence of the stiffness and of the elastic–plastic properties of the samples. KW - Atomic force microscope KW - Force-distance curves KW - Indentation KW - Elastic-plastic properties KW - Adhesion KW - Time-temperature superposition principle KW - Glass transition temperature PY - 2005 U6 - https://doi.org/10.1016/j.jcis.2005.09.043 SN - 0021-9797 SN - 1095-7103 SP - 1 EP - 8(?) PB - Elsevier CY - Orlando, Fla. AN - OPUS4-11187 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Döring, Joachim A1 - Stark, Wolfgang T1 - Ultrasonic Production Control N2 - Ultrasound waves penetrate solid objects without damaging them. Their fields of application range from the imaging of internal organs in medicine, to interior testing of mechanical and chemical engineering components. However, ultrasonic systems can also be used to visualise the way the mechanical properties of reactive resins change during processing in the mould. PY - 2001 SN - 0945-0084 VL - 91 IS - 1 SP - 35 EP - 36 PB - Hanser CY - München AN - OPUS4-2135 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Döring, Joachim A1 - Stark, Wolfgang T1 - Produktionskontrolle mit Ultraschall N2 - Ultraschallwellen durchdringen Festkörper, ohne sie zu schädigen. Der Einsatzbereich von Ultraschall reicht von der Darstellung der inneren Organe in der Medizin bis zur Prüfung des Inneren von Bauteilen im Maschinen- und Anlagenbau. Ultraschall-Systeme können jedoch auch genutzt werden, um sichtbar zu machen, wie sich mechanische Eigenschaften von Reaktionsharzen während ihrer Verarbeitung im Werkzeug verändern. PY - 2001 UR - http://www.kunststoffe.de/directlink.asp?KU101838 SN - 0023-5563 VL - 91 IS - 1 SP - 83 EP - 85 PB - Hanser CY - München AN - OPUS4-2137 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Döring, Joachim A1 - Stark, Wolfgang A1 - Bartusch, Jürgen A1 - Mc Hugh, Jarlath T1 - Contribution to ultrasound cure control for composite manufacturing N2 - The curing conditions play an important role in the quality assurance of composite products. Especially as composite materials are widely used in high tech areas so that they are required to fulfil high quality Standards. Some problems which occur during curing, for instance undercuring, can hardly be detected using Standard NDT investigations, mainly because they are manifested only at high temperatures, particularly close to glass-rubber-transition. On-line eure monitoring has the outstanding advantage that it can monitor the material parameters even at the highest temperatures possible. In recent years eure monitoring with ultrasonic methods has become more populär. In comparison to dielectric methods mechanical parameters are measured directly. The quantities to be measured are the velocity and the attenuation of the sound wave. On this basis the storage and loss modulus can be calculated. Depending on the form of excitation with longitudinal or transversal waves these moduli are referred to as long wave or shear modulus. Well developed Computer based technology and sensor materials are available in the non-destructive testing (NDT) market. The measuring equipment employed a commercial NDT System, which worked computer-aided. With a special Software the demands of automatic Operation under industrial conditions was accomplished. This measurement equipment was tested on composites. Its structure, performance and some practical results will be presented in the following paper. T2 - 15th World Conference on Non-Destructive Testing (WCNDT) CY - Roma, Italy DA - 15.10.2000 PY - 2000 UR - http://www.ndt.net/article/wcndt00/papers/idn482/idn482.htm SN - 1435-4934 VL - 5 IS - 11 PB - NDT.net CY - Kirchwald AN - OPUS4-2136 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Döring, Joachim A1 - Stark, Wolfgang A1 - Bartusch, Jürgen A1 - Mc Hugh, Jarlath A1 - Simon, W. T1 - Ultraschall-Prozesskontrolle mechanischer Parameter von aushärtenden Polymeren - Inline-Sensorik für die Herstellung von Kunststoffkomponenten KW - Aushärtung KW - Ultraschall KW - Sensoren KW - Materialparameter PY - 2007 SN - 0025-5300 VL - 49 IS - 5 SP - 238 EP - 242 PB - Hanser CY - München AN - OPUS4-14976 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Döring, Joachim A1 - Stark, Wolfgang A1 - Mc Hugh, Jarlath A1 - Bartusch, Jürgen T1 - Ultrasound on-line cure monitoring for industrial applications N2 - In recent years eure monitoring with ultrasonic methods became more important. An on-line measurement System for industrial applications is presented in this paper. It operates in through-transmission and the measured parameters are the sound velocity and the attenuation of the sound wave. An objective of this paper is to establish the ränge of possible applications for an ultrasonic eure monitoring System. KW - Ultrasonic monitoring KW - Cure process KW - Composite material KW - Process controlling PY - 2000 SN - 0963-6935 PB - Woodhead Publ. CY - Cambridge AN - OPUS4-1061 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fengler, Petra A1 - Stark, Wolfgang A1 - Döring, Joachim A1 - Mc Hugh, Jarlath T1 - Coupling of hidden ultrasound sensors to a moulding tool N2 - Ultrasound on-line NDT methods have been demonstrated as a useful tool for monitoring the curing reaction of thermosets. In order to achieve this ultrasound sensors are incorporated into compression, injection and RTM (resin transfer) mould. For many commercial products imprints or any surface markings upon the moulded product are undesirable. Due to its physical properties ultrasound has a large advantage over other techniques for similar applications. The sound wave can pass through the wall of the mould and direct contact with the moulded part is not required. In this particular case one fundamental problem is a good coupling of the sensors to the mould wall. Several mediums came into question but because of the high technical (e. g. temperature and long time stability) and practical demands, it was decided that dry (non-fluid) coupling would be the most promising candidate. A handful of coupling foils suitable also at high temperatures and for long time application under industrial conditions were tested and are presented in this paper. KW - Sensors KW - Ultrasound KW - Mould wall coupling KW - Thermoset manufacturing PY - 2004 UR - http://www.ndt.net/article/v09n03/stark/stark.htm SN - 1435-4934 VL - 9 IS - 3 SP - 1 EP - 10 PB - NDT.net CY - Kirchwald AN - OPUS4-3316 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 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 - Hoster, B. A1 - Jaunich, Matthias A1 - Stark, Wolfgang T1 - Monitoring of the vulcanisation process by ultrasound during injection moulding N2 - Today rubber is due to its unique property profile one of the most important materials for the production of bearings, dampers or also tires and tubes. In the production of rubber goods a chemical cross-linking reaction (vulcanisation) generates the final material properties. This process takes place during the shape giving of the rubber compound in the mould and can proceed for several minutes. The cross-linking process is influenced by the mixture of the basic polymer, the cross-linking agent, the influence of catalysts and inhibitors and especially the processing conditions. The quality of every ingredient, the reproducibility of the mixing ratio, the homogeneity of the mixture and the accurateness in temperature control can have a direct influence on the cross linking reaction. To control the quality of a rubber compound and verify the processing conditions in industry moving die rheometers, named curemeter, are involved in the production process. Starting from our experience in cure monitoring of thermosetting materials by measuring ultrasound velocity in the mould we extended the measuring principle to rubber vulcanisation monitoring. After first investigations using a compression mould we dealt here with on-line monitoring of vulcanisation in an injection moulding process which is one of the most used techniques in rubber industry. KW - Ultrasonic KW - Sound velocity KW - Vulcanisation KW - On-line monitoring KW - Injection moulding PY - 2009 UR - https://www.ndt.net/search/docs.php3?id=8042 SN - 1435-4934 VL - 14 IS - 9 SP - 1 EP - 9 PB - NDT.net CY - Kirchwald AN - OPUS4-19858 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jaunich, Matthias A1 - Stark, Wolfgang T1 - Monitoring the vulcanization of rubber with ultrasound: Influence of material thickness and temperature N2 - In consideration of the influence of the curing reaction on the material properties of elastomers, it is very important to control the vulcanization process properly. As shown previously [1], the effects of the vulcanization reaction of an elastomer can be monitored by use of ultrasonic sound waves. This technique has to a certain degree a high similarity to the standard curemeter test according to ISO 6502 but can be applied also inside a production tool. So far, the method was only applied to the vulcanization of one compound at a given temperature and sample thickness. This is now complemented with measurements on another compound system at different temperatures and sample thicknesses. The expected effects of temperature and thickness on the curing behaviour were found by use of the ultrasound online control. KW - Vulcanization KW - Cure process KW - Ultrasound KW - Curemeter KW - Elastomer KW - Natural rubber PY - 2009 U6 - https://doi.org/10.1016/j.polymertesting.2009.08.006 SN - 0142-9418 VL - 28 IS - 8 SP - 901 EP - 906 PB - Elsevier Science CY - Amsterdam [u.a.] AN - OPUS4-19959 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jaunich, Matthias A1 - Stark, Wolfgang T1 - Einfluss der Härtung auf die Materialeigenschaften eines Harnstoffharzes N2 - Über die in der Technik weit verbreitete typisierte Harnstoffformmasse UF 131.5, ein Aminoplast, wird berichtet, dass sie im Zuge der thermisch aktivierten Vernetzungsreaktion wegen "Überhärtung" mangelhafte Eigenschaften annimmt. Zur Verifizierung dieses Effektes werden mithilfe der Ultraschall-Prozesskontrolle gezielt Proben unterschiedlicher Aushärtegrade hergestellt. Sie werden mit verschiedenen Methoden, wie der "Kochprobe" und der Thermoanalyse, charakterisiert und auf ihre Materialeigenschaften untersucht. Dabei zeigt sich ein deutlicher Einfluss der Härtezeit auf die Glasübergangstemperatur der Formmasse. In den mechanischen Eigenschaften ist eine Veränderung allerdings nur in der Schlagzähigkeit festzustellen, die sich mit steigender Härtezeit sogar wesentlich verbessert. PY - 2009 SN - 0025-5300 VL - 51 IS - 11-12 SP - 828 EP - 834 PB - Hanser CY - München AN - OPUS4-20566 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jaunich, Matthias A1 - Stark, Wolfgang A1 - Hoster, B. T1 - Monitoring the vulcanization of elastomers: Comparison of curemeter and ultrasonic online control N2 - The vulcanization of elastomeric materials has a high impact on the properties of the final product. Therefore, it is important to monitor and control this crosslinking process. A common technique to attain the necessary curing time is the use of a curemeter in accordance with ISO 6502 in order to determine the time for full cure of a sample with a standardized geometry. Based on this result and a lot of practical experience, the required curing time for a given product geometry is estimated. Within the scope of this work, a new analysis technique will be compared with the standard procedure. The ultrasonic online control employs ultrasound waves to measure the changes in material properties caused by vulcanization. For this study, a natural rubber compound with a conventional curing system was investigated by both techniques. It was found that the results of the ultrasonic technique show good agreement with the results of the curemeter. KW - Cure process KW - Ultrasound KW - Curemeter KW - Elastomer KW - Vulcanization KW - Online control PY - 2009 U6 - https://doi.org/10.1016/j.polymertesting.2008.11.005 SN - 0142-9418 VL - 28 IS - 1 SP - 84 EP - 88 PB - Elsevier Science CY - Amsterdam [u.a.] AN - OPUS4-18674 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jaunich, Matthias A1 - Stark, Wolfgang A1 - Wolff, Dietmar T1 - Comparison of low temperature properties of different elastomer materials investigated by a new method for compression set measurement N2 - The method for the determination of compression set values with a Dynamic Mechanical Analysis (DMA) setup at low temperatures, which was presented previously, allows a much faster and readily automated procedure than the standardized compression set test according to ISO 815-2. This method is applied to a series of different elastomeric materials that are commonly used for sealing applications. The results of the compression set test are compared with results from thermal analysis to allow an in depth comparison of the material behaviour at low temperatures. Furthermore, a comparison between two EPDM materials is presented. These materials show very similar properties determined by thermo analytical methods such as Differential Scanning Calorimetry (DSC) and Dynamic Mechanical Analysis (DMA) but differ clearly in their compression set behaviour. This comparison shows the importance and value of information of the compression set test in addition to thermal analysis to judge the behaviour of sealing materials and confirms the relevance of the new compression set test method for the investigation of low temperature properties of elastomers. KW - Sealing material KW - Elastomer KW - Compression set KW - Dynamic mechanical analysis KW - Low temperature behaviour PY - 2012 U6 - https://doi.org/10.1016/j.polymertesting.2012.07.016 SN - 0142-9418 VL - 31 IS - 8 SP - 987 EP - 992 PB - Elsevier Science CY - Amsterdam [u.a.] AN - OPUS4-26538 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 - Jaunich, Matthias A1 - Stark, Wolfgang A1 - Wolff, Dietmar T1 - A new method to evaluate the low temperature function of rubber sealing materials N2 - A new method for the evaluation of the low temperature properties of rubber materials is presented. The method emulates the standardized compression set measurement, which is frequently used for sealing materials, but can be performed within a considerably shorter time. The results are compared with the standard test and found to be qualitatively the same. Slight differences are discussed on the basis of the differences in the measurement procedures. Further data evaluation is done by fitting functions to describe the material behaviour. KW - Sealing material KW - Elastomer KW - Compression set KW - Dynamic mechanical analysis KW - Low temperature behaviour PY - 2010 U6 - https://doi.org/10.1016/j.polymertesting.2010.07.006 SN - 0142-9418 VL - 29 IS - 7 SP - 815 EP - 823 PB - Elsevier Science CY - Amsterdam [u.a.] AN - OPUS4-21914 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jaunich, Matthias A1 - Stark, Wolfgang A1 - Wolff, Dietmar T1 - Low temperature properties of rubber seals N2 - Rubber is widely used as sealing material in various applications. In many fields the sealing function at low temperatures is necessary. Therefore the understanding of failure mechanisms is of high importance. Rubbers are normally used above their glass-rubber transition region but the minimum working temperature limit is not defined precisely. Therefore the lower operation temperature limit of rubber seals should be determined in dependence of the material properties. The results of Differential Scanning Calorimetry (DSC) and Dynamic Mechanical Analysis (DMA) are combined with the results of the standardized compression set according to ISO 815 respectively a modified test using the DMA equipment. N2 - Tiefentemperaturverhalten von Elastomerdichtungen Elastomere werden vielfach als Dichtungsmaterial für verschiedene Anwendungen eingesetzt. In vielen Bereichen ist die Funktion der Dichtung auch bei tiefen Temperaturen erforderlich. Daher ist das Verständnis des Versagensmechanismus von großer Bedeutung. Normalerweise werden Elastomere oberhalb ihres Glass-Gummi Übergangsbereiches eingesetzt aber die minimale Einsatztemperatur ist nicht exakt definiert. Daher ist es sinnvoll diese untere Temperatureinsatzgrenze in Abhängigkeit von den Materialeigenschaften zu bestimmen. Die Ergebnisse der DSC und der DMA werden mit den Ergebnissen des standardisierten Druckverformungsrestes nach ISO 815 und einer abgewandelten Messung mit der DMA kombiniert. KW - Sealing material KW - Elastomer KW - Compression set KW - Dynamic mechanical analysis KW - Low temperature behaviour PY - 2011 SN - 0948-3276 SN - 0022-9520 IS - 03 SP - 52 EP - 55 PB - Hüthig CY - Heidelberg AN - OPUS4-23422 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jaunich, Matthias A1 - von der Ehe, Kerstin A1 - Wolff, Dietmar A1 - Völzke, Holger A1 - Stark, Wolfgang T1 - Understanding low temperature properties of elastomer seals N2 - Elastomers are widely used as the main sealing materials for containers for low and intermediate level radioactive waste and as an additional component to metal seals in spent fuel and high active waste containers. The safe encapsulation of the radioactive container inventory has to be guaranteed according to regulation and appropriate guidelines for long term storage periods as well as for temperatures as low as -40°C during transport. Therefore, the understanding of failure mechanisms that lead to leakage at low temperatures is of high importance. It is known that the material properties of elastomers are strongly temperature dependent. At low temperatures, this is caused by the rubber-glass transition (abbreviated: glass transition). During continuous cooling, the material changes from a rubber-like entropy elastic to a stiff energy elastic behaviour, which allows nearly no strain or retraction. Hence, rubbers are normally used above their glass transition, but the minimum working temperature limit is not defined precisely; this can cause problems during the above noted applications. Therefore, the lower operation temperature limit of elastomer seals must be determined in dependence of the material properties. Differential scanning calorimetry (DSC) and dynamic mechanical analysis (DMA) are combined with standardised measurements to determine the compression set according to ISO 815. To reduce the test time of the standard tests, a faster technique than normally used was developed. Additionally, the breakdown temperature of the sealing function of complete O ring seals was measured in a component test set-up to compare it with the results of the other tests. The experimental set-up is capable of measuring the leakage rate at low temperatures by the pressure rise method. A fluorocarbon rubber (FKM) was selected for this investigation as it is often used for radioactive waste containers. The materials (seals and test sheets) were purchased from a commercial seal producer. KW - Sealing material KW - Elastomer KW - Compression set KW - Dynamic mechanical analysis KW - Low temperature behaviour PY - 2011 U6 - https://doi.org/10.1179/1746510911Y.0000000004 SN - 1746-5095 SN - 1746-5109 SN - 0957-476X VL - 22 IS - 2 SP - 83 EP - 88 PB - Ramtrans Publ. CY - Ashford AN - OPUS4-24015 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jaunich, Matthias A1 - Wolff, Dietmar A1 - Stark, Wolfgang T1 - Low temperature properties of rubber seals - Results of component tests - N2 - Rubbers are widely used as sealing material in various applications. In many fieldsthefunction of seal materials at lowtemperatures is required. Therefore the understanding of faiiure mechanisms that lead to leakage at low temperatures is of high importance. Therefore the lower Operation temperature limit of rubber seals should be determined in dependence of the material properties. The results of Differential Scanning Calorimetry (DSC) and Dynamic Mechanical Analysis (DMA) are combined with results of standardized measurements as the compression set according to ISO 815. To reduce the test time of the Standard tests a faster and more efficient technique was developed and applied. In addition the breakdown temperature of the sealing function of O-ring seals at lowtemperatures is measured in a component test Setup in dependence of the material and the degree of compression. KW - Seal KW - O-ring KW - Low temperature KW - Component test KW - Compression set KW - Dichtungen KW - O-Ringe KW - Tiefe Temperatur KW - Bauteilversuche KW - Druckverformungsrest PY - 2013 SN - 0948-3276 SN - 0022-9520 VL - 66 IS - 7-8 SP - 26 EP - 30 PB - Hüthig CY - Heidelberg AN - OPUS4-28894 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kelm, Jürgen A1 - Stark, Wolfgang A1 - Bovtun, V. A1 - Borisov, V. A1 - Yakimenko, Y. T1 - Investigation of Crosslinking Process in Thermosets and Elastomers by Microwave Methods - Basic Study for the Monitoring Method Development KW - Dielectric parameters KW - Microwave methods KW - Crosslinking KW - Cure KW - Vulcanisation KW - Thermosets KW - Elastomers KW - Monitoring PY - 2000 SN - 0025-5300 PB - Carl Hanser Verlag CY - München AN - OPUS4-1053 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Krüger, Simone A1 - Stark, Wolfgang A1 - Goering, Harald A1 - Michel, Uwe T1 - Thermoanalyse der Phenolharzhärtung - Ein Weg zur Optimierung der Nachtemperung N2 - Angesichts der spezifischen Bedeutung der Aushärtung von Phenolharzen für ihre Eigenschaften als Ingenieurwerkstoffe besteht großes Interesse an deren quantitativer Charakterisierung. Mittels DSC-Messungen unter hohem Druck (HP-DSC) kann die Vernetzungsreaktion der Phenolharzformmassen durch die Unterdrückung der Verdampfung niedermolekularer Substanzen ohne störende Überlagerungen verfolgt werden. Mittels verschiedener Vernetzungsgrade können die Einflussparameter der Aufheizrate und der Nachtemperung optimiert werden. Die Messergebnisse ermöglichen eine Modellierung der Reaktionskinetik mit dem Ziel einer verbesserten Prozessführung und Qualitätskontrolle in der industriellen Praxis. KW - Phenolharze KW - Thermische Analyse KW - DMA KW - DSC KW - Aushärtung KW - Glasübergang PY - 2006 SN - 0025-5300 VL - 48 IS - 11-12 SP - 556 EP - 561 PB - Carl Hanser Verlag CY - München AN - OPUS4-13802 LA - deu 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 U6 - 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 - 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 - Mielke, Werner A1 - Stark, Wolfgang T1 - Unter Kontrolle - Aushärtung duroplastischer Formmassen PY - 1995 SN - 0047-3766 VL - 29 SP - 35 EP - 37 PB - Verl. Moderne Industrie CY - Landsberg AN - OPUS4-11798 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Munz, Martin A1 - Sturm, Heinz A1 - Stark, Wolfgang T1 - Mechanical gradient interphase by interdiffusion and antiplasticisation effect - study of an epoxy/thermoplastic system N2 - A stoichiometric amine–epoxy formulation was cured in the presence of a thermoplastic, namely poly(vinylpyrrolidone) (PVP). The epoxy system consisted of the resin diglycidyl ether of bisphenol A (DGEBA) and the aromatic curing agent 4,4'-diaminodiphenylsulfone (DDS). As shown for this system in a former study by Oyama et al. [Oyama HT, Lesko JJ, Wightman JP. J Polym Sci B 1997;35:331–46. [36]], preferential absorption of amine molecules by PVP can occur. In the present study, the focus is on the variations of local elastic properties within the epoxy interphase adjacent to the PVP layer. The curing was performed close to the glass transition temperature, Tα, of the PVP film, namely at 170 °C. Variations of the local amine concentration were tracked using energy-dispersive analysis of X-rays (EDX), by taking benefit of the sulfur contained in DDS. Using temperature-dependent dynamic mechanical analysis (DMA), a series of epoxy reference samples of different amine–epoxy concentration ratios, r, was investigated in order to work out the relationship between r and the epoxy storage modulus at room temperature. In the excess-epoxy regime, r<1, the modulus is observed to increase with departure from the stoichiometric ratio, r=1. Considering the respective suppression of the ß-transition, the observed characteristic can be explained by an antiplasticisation effect. Depth-sensing indentation (DSI) experiments across the epoxy/PVP interphase provided evidence for strong modulus variations. In consistency with the EDX and the DMA data, in the vicinity of the PVP layer the local epoxy modulus is increased. The total change of the epoxy Young's modulus is ~1.1 GPa. However, the total width of the modulus decay of ~175 µm is ~2.5 times larger than the one of the DDS concentration gradient. This finding is discussed in terms of additional spatial variations of the DGEBA concentration as well as long-range diffusion currents of DDS induced by the interdiffusion processes and their effect on the final network of crosslinks. KW - Interdiffusion KW - Interphase/interface KW - Polymer PY - 2005 U6 - https://doi.org/10.1016/j.polymer.2005.06.098 SN - 0032-3861 SN - 1873-2291 VL - 46 IS - 21 SP - 9097 EP - 9112 PB - Springer CY - Berlin AN - OPUS4-10893 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rabe, Torsten A1 - Eberlee, Ina A1 - Güther, Wolfgang A1 - Stark, Wolfgang T1 - Mechanische und thermomechanische Charakterisierung keramischer Grünfolien KW - Keramische Grünfolien KW - Mechanische Prüfung KW - DMTA PY - 2004 SN - 0173-9913 SN - 0196-6219 VL - 18 IS - 1 SP - 58 EP - 68 PB - Göller CY - Baden-Baden AN - OPUS4-5338 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schulze, Dietmar A1 - Fengler, Petra A1 - Stark, Wolfgang T1 - Die Ermittlung von Ozonkonzentrationen bei der Prüfung der Ozonbeständigkeit von Elastomeren N2 - Dargestellt wird eine Gegenüberstellung der Ergebnisse von Messungen zur Ozonkonzentrationsbestimmung nach zwei Verfahren. International wird in der Kautschukindustrie ein UV-spektroskopisches Verfahren angewandt. Die deutsche Kautschukindustrie verwendet ein nasschemisches Verfahren. Die beiden Verfahren ergeben nicht die gleichen Ergebnisse. Daher wird der Unterschied genauer ermittelt. Die Auswirkungen der unterschiedlichen Ozonkonzentrationsbestimmungen auf die Prüfung der Ozonbeständigkeit an Elastomeren werden gezeigt. KW - Ozonkonzentrationsbestimmung KW - UV-Spektroskopie KW - Nasschemische Analyse KW - Ozonbeständigkeit KW - Elastomere PY - 2011 SN - 0948-3276 SN - 0022-9520 VL - 05 SP - 15 EP - 19 PB - Hüthig CY - Heidelberg AN - OPUS4-23832 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stark, Wolfgang T1 - Investigation of the curing behaviour of carbon fibre epoxy prepreg by dynamic mechanical analysis DMA N2 - Carbon fibre prepregs have found widespread application in lightweight constructions. They are based on a carbon fibre fabric impregnated with reactive epoxy resin. Measurements were carried out using commercially available prepreg material. For Dynamic Mechanical Analysis (DMA), a single cantilever measuring device was applied. The DMA results were refined by additional DSC measurements. The measurements were carried out with dynamic heating in the temperature range -90 to 280 °C. The heating rates were 1 and 2 K/min, respectively. A glass transition of the uncured material (Tg0) near 1 °C, and crosslinking-induced vitrification and devitrification at the maximal glass transition temperature of the cured material (Tgmax) in the temperature range 220 to 230 °C were found. The activation energies for the glass transitions were determined using an Arrhenius plot. By detailed consideration of the influence of the frequency on the DMA data, indications for gelation were deduced. KW - CRP KW - Prepreg KW - Carbon fibre KW - Epoxy KW - DMA KW - DSC KW - Glass transition KW - Crosslinking KW - Vitrification KW - Devitrification PY - 2013 U6 - https://doi.org/10.1016/j.polymertesting.2012.11.004 SN - 0142-9418 VL - 32 IS - 2 SP - 231 EP - 239 PB - Elsevier Science CY - Amsterdam [u.a.] AN - OPUS4-27584 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stark, Wolfgang T1 - Entwicklung der Gütesicherung bei Isolierstoffen KW - Materialprüfungsamt KW - Kunstharze KW - Bakelit KW - Phenolharz KW - Aminoharz KW - Gütesicherung KW - Technische Vereinigung PY - 2010 UR - https://www.google.de/url?sa=t&rct=j&q=&esrc=s&source=web&cd=1&ved=0ahUKEwivis-l7tvKAhVFWBoKHa-jD1gQFggeMAA&url=https%3A%2F%2Fwww.kunststoffe.de%2F_storage%2Fasset%2F538701%2Fstorage%2Fmaster%2Ffile%2F5804889%2Fdownload%2FEntwicklung%2520der%2520G%25C3%25BCtesicherung%2520bei%2520Isolierstoffen.pdf&usg=AFQjCNE14vu5Aw1foQ7OZdcTT2vwsRX_TQ SN - 0023-5563 VL - 100 IS - 2 SP - 14 EP - 17 PB - Hanser CY - München AN - OPUS4-20935 LA - deu 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 U6 - 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 - 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 - Döring, Joachim A1 - Kelm, Jürgen T1 - Ultraschall on-line Prozesskontrolle bei der Vulkanisation KW - Prozesskontrolle KW - Vulkanisation KW - Ultraschall KW - Sensoren KW - Schubmodul KW - Verlustmodul PY - 2000 SN - 0948-3276 SN - 0022-9520 SP - 9 Seiten PB - Hüthig CY - Heidelberg AN - OPUS4-997 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stark, Wolfgang A1 - Döring, Joachim A1 - Kürten, C. T1 - Vernetzung reaktiver Kunststoffe mit Ultraschall überwachen KW - Elastomer KW - Epoxidharz KW - Phenolharz KW - Vernetzung KW - Vulkanisation KW - Schallgeschwindgkeit KW - Prozesskontrolle PY - 2008 SN - 0939-2629 SN - 0176-6058 IS - 2 SP - 31 EP - 33 PB - Holzverl. CY - Kissing AN - OPUS4-17587 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stark, Wolfgang A1 - Döring, Joachim A1 - Walentowski, Heinz-Ulrich T1 - Crosslinking Instead of Glassy Transition N2 - In processing fibre-reinforced composites, the curing reaction can be significantly retarded if the temperature and reaction time are not optimally set. In such situations, complete curing is sometimes impossible under practically relevant conditions. It is difficult for processors to recognize or detect incomplete curing. The equilibrium glass transition temperature plays an important role in complete curing in the production process. PY - 2000 SN - 0945-0084 VL - 90 IS - 4 SP - 33 EP - 35 PB - Hanser CY - München AN - OPUS4-822 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stark, Wolfgang A1 - Döring, Joachim A1 - Walentowski, Heinz-Ulrich T1 - Vernetzen statt Verglasen PY - 2000 UR - http://www.kunststoffe.de/ku/default.asp SN - 0023-5563 VL - 90 IS - 4 SP - 90 EP - 92 PB - Hanser CY - München AN - OPUS4-823 LA - deu 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 U6 - 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 A1 - Hoster, B. A1 - Kürten, C. T1 - Längenänderung bei erhöhten Temperaturen und Aushärtegrad von duroplastischen Formteilen KW - Harnstoffharze KW - Verzug KW - Spritzgießen KW - Aushärtegrad KW - Schrumpf PY - 2006 SN - 0176-1625 VL - 59 IS - 10 SP - 627 EP - 631 PB - Gupta CY - Ratingen AN - OPUS4-14444 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stark, Wolfgang A1 - Hoster, B. A1 - Kürten, Ch. T1 - Nachtemperung von duroplastischen Bauteilen - Spagat zwischen Eigenschaftsverbesserung und Eigenschaftsverschlechterung PY - 2005 SN - 0176-1625 VL - 58 IS - 11 SP - 718 EP - 722 PB - Gupta CY - Ratingen AN - OPUS4-11592 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stark, Wolfgang A1 - Jaunich, Matthias T1 - Investigation of ethylene/vinyl acetate copolymer (EVA) by thermal analysis DSC and DMA N2 - Two types of commercially applied Ethylene/Vinyl Acetate Copolymers (EVA) for encapsulation of photovoltaic modules were investigated by the thermal analysis methods of Differential Scanning Calorimetry (DSC) and Dynamic Mechanical Analysis (DMA) in the temperature range from -150 °C to 200 °C. Glass transition, crystal melting and cross-linking were analyzed. The aims of the investigations were to gain more information for incoming goods control and to get information about the whole temperature dependent material properties in the investigated temperature range, starting at very low temperatures up to the crosslinking temperature region. KW - EVA KW - Thermal analysis KW - DSC KW - DMA KW - Glass transition KW - Crystal melting KW - Cross-linking PY - 2011 U6 - https://doi.org/10.1016/j.polymertesting.2010.12.003 SN - 0142-9418 VL - 30 IS - 2 SP - 236 EP - 242 PB - Elsevier Ltd. CY - Amsterdam [u.a.] AN - OPUS4-23206 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stark, Wolfgang A1 - Jaunich, Matthias T1 - Thermoanalytische Charakterisierung von Ethylen-Vinylacetat-Copolymer (EVA) für Photovoltaikmodule N2 - Das Ziel der Untersuchungen war mit Hilfe von DSC und DMA EVA-Folien im Anlieferungszustand hinsichtlich der Lage der Glasübergangstemperatur, des Schmelzverhaltens und der Temperaturabhängigkeit der Vernetzungsreaktion zu charakterisieren. Auf dieser Basis sollte die Lieferstabilität im Sinne einer Wareneingangskontrolle auf eine messtechnische Basis gestellt werden. In einem 2. Schritt sollte die vernetzte Folie dahingehend charakterisiert werden, ob infolge der Vernetzung eine Änderung der KW - Photovoltaik KW - Klebfolie KW - EVA KW - DSC KW - DMA PY - 2011 VL - 8 SP - 3 EP - 5 AN - OPUS4-24168 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stark, Wolfgang A1 - Jaunich, Matthias A1 - Bohmeyer, W. A1 - Lange, K. T1 - Investigation of the crosslinking behaviour of ehtylene vinyl acetate (EVA) for solar cell encapsulation by rheology and ultrasound N2 - EVA is a widely used material for the encapsulation of photovoltaic modules. It melts at elevated temperatures, and seals the module before it is crosslinked at temperatures above 130 °C by a peroxide-initiated crosslinking reaction. EVA has good optical properties necessary for application in solar modules. For process optimization and quality management, a method for the quick and reliable characterization of EVA crosslinking behaviour is of great value. Here, the practicability of ultrasound for online crosslinking monitoring is demonstrated. A sound velocity increase of about 8 m/s during the crosslinking reaction is found. The ultrasound results are compared with rheometer measurements performed with a curemeter typically used for the investigation of rubber crosslinking. KW - Ethylene vinyl acetate KW - EVA KW - Crosslinking KW - Ultrasound KW - Rheology KW - Curemeter KW - DSC PY - 2012 U6 - https://doi.org/10.1016/j.polymertesting.2012.07.004 SN - 0142-9418 VL - 31 IS - 7 SP - 904 EP - 908 PB - Elsevier Science CY - Amsterdam [u.a.] AN - OPUS4-26291 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 -