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 - 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 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 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 -