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 - 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 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 - McHugh, J. T1 - Cure state detection for pre-cured carbon-fibre epoxy prepreg (CFC) using temperature-modulated differential scanning calorimetry (TMDSC) N2 - Carbon-fibre prepregs have found widespread use in lightweight applications. They are based on a carbon-fibre fabric impregnated with reactive epoxy resin. Prepreg materials are generally pre-cured so that they have a higher molecular weight than typical resins in order to reduce resin flow, which facilitates storage and later processing properties. The measurements were carried out using commercially available materials and follow the published DMA investigations of the same material. TMDSC was used to find the correlation between curing conditions, the degree of cure and glass transition temperature. TMDSC has the advantage over standard DSC that it enables better determination of the glass transition temperature, which is often accompanied by an exothermic curing reaction, and thus overshadowed. The influence of the amplitude of temperature modulation was tested in preliminary experiments. For non-cured material a glass transition temperature of approximately 0 °C was determined; whereas for the totally cured material it was approximately 230 °C. The changes in degree of cure, temperature of actual glass transition and post-reaction are given as a function of curing time at 180 °C. The correlation between actual glass transition temperature and degree of cure is derived. KW - Prepreg KW - Carbon fibre KW - Glass transition KW - Degree of curing KW - DSC KW - TMDSC PY - 2013 U6 - https://doi.org/10.1016/j.polymertesting.2013.07.007 SN - 0142-9418 VL - 32 IS - 7 SP - 1261 EP - 1272 PB - Elsevier Science CY - Amsterdam [u.a.] AN - OPUS4-29067 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 - 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 - CHAP A1 - Stark, Wolfgang A1 - Bohmeyer, W. ED - Karbhari, V.M. T1 - Non-destructive evaluation (NDE) of composites: using ultrasound to monitor the curing of composites N2 - Typical composite materials for lightweight construction consist of a fibre (glass or carbon) reinforced thermosetting matrix. The impregnation of the fabric is made with liquid resin – usually epoxy resin or unsaturated polyester resin are used. The main processing methods are resin transfer moulding (RTM) and prepreg technology often used in combination with autoclave curing. After shaping, the resin must be cured. The final properties of the produced parts depend on the curing degree and the final glass transition temperature. Analytical methods and the use of ultrasound for online cure monitoring in the manufacturing process are introduced. Examples for the application of ultrasonic cure monitoring for the production of composite parts for traffic systems are also covered. KW - Epoxy KW - DSC KW - DMA KW - Kinetic KW - Autoclave KW - Curing KW - Glass transition KW - Curing behaviour KW - Curing degree KW - Rheology KW - Differential scanning calorimetry KW - Dynamic mechanical analysis KW - Sound velocity KW - Sound damping KW - Resin transfer moulding KW - RTM KW - Prepreg PY - 2013 SN - 978-0-85709-344-8 SN - 978-0-85709-355-4 U6 - https://doi.org/10.1533/9780857093554.1.136 SN - 2052-5281 SN - 2052-529X N1 - Serientitel: Woodhead publishing sereies in composites science and engineering – Series title: Woodhead publishing sereies in composites science and engineering VL - 43 IS - Part 1 / Chapter 7 SP - 136 EP - 181 PB - Woodhead Publishing Ltd CY - Cambridge, UK AN - OPUS4-28848 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stark, Wolfgang A1 - Jaunich, Matthias A1 - McHugh, J. T1 - Carbon-fibre epoxy prepreg (CFC) curing in an autoclave analogue process controlled 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. DMA measurements under temperature conditions similar to an autoclave programme were carried out using commercially available prepreg material with a high glass transition temperature. The characteristic of the temperature programme was a dynamic heating segment at 1.5 K/min followed by a longer isothermal segment at 180 °C. The courses of the storage modulus E', loss modulus E'' and tanδ were recorded. The measuring frequency was varied between 1 Hz and 33.3 Hz. Gelation and vitrification are assigned. The influence of the measuring frequency on the time to vitrification and the correlation with DSC are discussed. The reaction does not end even after 10 h curing at 180 °C, which is interpreted as the slow cessation of the reaction caused by vitrification. KW - Prepreg KW - CFC KW - Curing KW - DMA KW - DSC KW - Autoclave KW - Gelation KW - Vitrification KW - Glass transition PY - 2013 U6 - https://doi.org/10.1016/j.polymertesting.2013.09.014 SN - 0142-9418 VL - 32 IS - 8 SP - 1487 EP - 1494 PB - Elsevier Science CY - Amsterdam [u.a.] AN - OPUS4-29479 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 -