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 DO - 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 - CONF A1 - Stark, Wolfgang T1 - Kinetic Model for Cross-linking Reaction of Epoxy Resin for Rotor Blade Production T2 - Thermosets Conference 2013 - From Monomers to Components CY - Berlin, Germany DA - 2013-09-18 PY - 2013 AN - OPUS4-28701 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 - 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 - 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 - 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 - 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, 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 - GEN A1 - Gorokhovatsky, Y.A. A1 - Krüger, Simone A1 - Brademann-Jock, Kerstin A1 - Stark, Wolfgang A1 - Temnov, Dmitri A1 - Kuvshinova, Oksana A1 - Goldade, V.A. ED - Fleming, R. J. T1 - Thermally stimulated luminescence in LDPE fibers T2 - 11th International Symposium on Electrets (ISE 11) CY - Melbourne, Australia DA - 2002-10-01 PY - 2002 SN - 0-7803-7560-2 SP - 138 EP - 140 PB - IEEE Service Center CY - Piscataway, NJ AN - OPUS4-1654 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Stark, Wolfgang A1 - Döring, Joachim A1 - Kelm, Jürgen A1 - Fritsch, Sebastian T1 - Kontrolle der Kautschukvulkanisation im Werkzeug mit Ultraschall N2 - Zusammenfassung In diesem Beitrag wird zunächst die für die on-line Prozesskontrolle an duroplastischen Formmassen entwickelte Ultraschallmesstechnik vorgestellt. Die Methode basiert auf der Durchschallung des vernetzenden Materials mit Hilfe von in das Werkzeug integrierten druck- und temperaturfesten 4 MHz-Ultraschallsensoren. Die Auswertung von Schalllaufzeit und Signalamplitude erfolgt vollautomatisch und dient der Berechnung von Schallgeschwindigkeit und -dämpfung. Beide Größen repräsentieren die änderung der mechanischen Eigenschaften infolge der Vernetzungsreaktion. Durch Anwendung auf vulkanisierende Materialien sollte die Anwendbarkeit der bewährten Methode erweitert werden. Im Ergebnis wird gezeigt, dass die Größe des Messeffekts von der Menge an Vernetzer (Schwefelkonzentration) abhängt. Bei ausreichend hohem Vernetzungsgrad zeigt die Ultraschallgeschwindigkeit signifikante, gut auswertbare Resultate, die den Ablauf der Vulkanisation on-line zu verfolgen gestatten. Ein Vergleich mit Vulkameterkurven zeigt große ähnlichkeiten und berechtigt zu der Hoffnung, dass die Methode industriellen Einsatz finden kann. T2 - Jahrestagung Zerstörungsfreie Materialprüfung 2002 CY - Weimar, Deutschland DA - 2002-05-06 KW - Prozesskontrolle KW - Vulkanisation KW - Vulkameter KW - Ultraschall KW - Schallgeschwindigkeit PY - 2002 UR - http://www.ndt.net/article/dgzfp02/papers/p21/p21.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 - OPUS4-1857 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Döring, Joachim A1 - Stark, Wolfgang A1 - Mc Hugh, Jarlath A1 - Bartusch, Jürgen A1 - Fengler, Petra T1 - Rheologische und akustische Bestimmung der Fließ-Härtungseigenschaften von Injektionsharzen N2 - Zusammenfassung Der Ausgangspunkt für diese Arbeiten ist eine in [1] beschriebene Ultraschall-(US)-Sensorik zur Aushärtungskontrolle. Sie wurde für rieselfähige Formmassen entwickelt [2,3]. Darauf aufbauend ist es das Ziel der vorliegenden Arbeit, die Voraussetzungen für den Einsatz dieser Sensorik beim Harzinjektionsverfahren zu schaffen und ihre Kalibrierung durch rheologische und DSC-Messungen zu ermöglichen. Der erste Teil des Beitrages beschäftigt sich mit dem technologischen Ablauf des Harzinjektionsverfahren und den Einsatzmöglichkeiten der US-Sensorik bei dieser Technologie. Ergebnisse von Schallgeschwindigkeits- und Dämpfungsmessungen für EP-Harze werden vorgestellt. Im zweiten Teil wird auf das Kalibrieren der US-Sensorik für den Verarbeiter eingegangen. Es kann mittels der bisherigen Prozessführung oder durch Vergleich mit den Ergebnissen anderer Mess-Verfahren wie Rheometer- oder Differential-Scanning-Calerometry-(DSC)-Messungen erfolgen. T2 - Jahrestagung Zerstörungsfreie Materialprüfung 2002 CY - Weimar, Deutschland DA - 2002-05-06 KW - Ultraschall KW - Harzinjektionsverfahren KW - RTM KW - Prozesskontrolle KW - Aushärtung PY - 2002 UR - http://www.ndt.net/article/dgzfp02/papers/v51/v51.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 - OPUS4-1913 LA - deu 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 - 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 DO - 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 - 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 - CONF A1 - Stark, Wolfgang T1 - Thermoanalytische Methoden DSC/Hochdruck-DSC und DMA bei der Charakterisierung der Vernetzung reaktiver Kunststoffe T2 - Praxistag Uni Rostock "Thermische Analyse für spezielle Anwendungen" CY - Rostock, Germany DA - 2012-06-19 PY - 2012 AN - OPUS4-26084 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stark, Wolfgang T1 - Characterization of thermosetting polymers for manufacturing of composite parts by thermal analysis methods T2 - 4th bilateral Symposium on heterocyclic and heterochain polymers for advanced materials CY - Iasi, Romania DA - 2012-09-03 PY - 2012 AN - OPUS4-26492 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stark, Wolfgang T1 - Charakterisierung der Vernetzungsreaktion von Harnstoff-Formmasse mittels Hochdruck-DSC T2 - 1. Wildauer Duromer-Tagung CY - Wildau, Germany DA - 2008-03-11 PY - 2008 AN - OPUS4-16720 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stark, Wolfgang T1 - Investigation the sealing behaviour of rubber seals at low temperatures T2 - 11. Schwarzheider Kunststoffkolloquium CY - Schwarzheide, Germany DA - 2011-09-21 PY - 2011 AN - OPUS4-24321 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Sturm, Heinz A1 - Schulz, Eckhard A1 - Stark, Wolfgang A1 - Bovtun, V. A1 - Friedrich, Jörg Florian ED - Olefjord, I. ED - Nyborg, L. ED - Briggs, D. T1 - Techniques for surface composition analysis with scanning force microscopy (SFM) using electrical surface properties T2 - 7th European Conference on Applications of Surface and Interface Analysis CY - Göteborg, Sweden DA - 1997-06-16 PY - 1997 SN - 0-471-97827-2 SP - 579 EP - 582 PB - Wiley CY - Chichester AN - OPUS4-6854 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Sturm, Heinz A1 - Stark, Wolfgang A1 - Bovtun, V. A1 - Schulz, Eckhard ED - Xia, Z. T1 - Methods for simultaneous measurements of topography and local electrical properties using scanning force microscopy N2 - Two different approaches to investigate the local complex conductivity and the surface charge with Scanning Force Microscopy (SFM) techniques are presented. It is shown that the measurement of local electrical properties with SFM leads to interesting information about the composition of electrically heterogeneous surfaces T2 - 9th International Symposium on Electrets (ISE 9) CY - Shanghai, China DA - 1996-09-25 PY - 1996 SN - 0-7803-2695-4 DO - https://doi.org/10.1109/ISE.1996.578073 SP - 223 EP - 228 PB - IEEE Service Center CY - Piscataway, NJ AN - OPUS4-6851 LA - eng 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 DO - 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 - GEN A1 - Schulz, Eckhard A1 - Sturm, Heinz A1 - Stark, Wolfgang A1 - Bovtun, V. ED - Xia, Z. T1 - Determination of electric properties of heterogeneous systems using the contact and noncontact scanning force microscopy (SFM) N2 - With an extended contact and non-contact mode scanning force microscope samples with different heterogeneous electrical properties can be characterized. The contact mode method allows the determination of local electric conductivities of heterogeneous systems at the sample surfaces. An interpretation of this behaviour can be obtained in combination with other SFM modes such as topography, friction and compliance used simultaneously. The non-contact mode SFM allows to get more information about the local surface charge of heterogeneous samples. In this paper two new SFM approaches will be discussed on examples of carbon-fibre reinforced, organic and ceramic materials T2 - 9th International Symposium on Electrets (ISE 9) CY - Shanghai, China DA - 1996-09-25 PY - 1996 SN - 0-7803-2695-4 DO - https://doi.org/10.1109/ISE.1996.578094 SP - 334 EP - 339 PB - IEEE Service Center CY - Piscataway, NJ AN - OPUS4-6852 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 DO - 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 -