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Stiffness variation in the interphase of amine-cured epoxy adjacent to copper microstructures
(2007)
In an effort to expand the understanding of the mechanical properties of the polymeric interphase on a metal surface, a composite consisting of epoxy and copper was prepared and analyzed. Scanning force microscopy-based force modulation microscopy (SFM-FMM) was employed along with dynamic mechanical analysis (DMA) and energy dispersive X-ray analysis (EDX). Diglycidyl ether of bisphenol A (DGEBA)-based epoxy resins were applied with amine curing agents. The samples were made taking advantage of electron beam lithography (EBL) in order to produce sharp edges of copper structures and a flat surface suitable for the SFM-FMM analysis, which was able to depict the stiffness within the interphase. It is considered significant information because the mechanical characteristic within the narrow interphase was revealed. Comparing with DMA and EDX, the stiffness information of SFM-FMM demonstrated a matching correlation and agreement in terms of preferential adsorption of the curing agent in the vicinity of the interface. The stiffness profiles of the two epoxy systems turned out to be different, and it shows the material dependence of the interphase characteristics.
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.
Determining a suitable and reliable end-of-lifetime criterion for O-ring seals is an important issue for long-term seal applications. Therefore, seal failure of ethylene propylene diene rubber (EPDM) and hydrogenated nitrile butadiene rubber (HNBR) O-rings aged in the compressed state at 125 °C and at 150 °C for up to 1.5 years was analyzed and investigated under static conditions, using both non-lubricated and lubricated seals. Changes of the material properties were analyzed with dynamic-mechanical analysis and permeability experiments. Indenter modulus measurements were used to investigate DLO effects. It became clear that O-rings can remain leak-tight under static conditions even when material properties have already degraded considerably, especially when adhesion effects are encountered. As a feasible and reliable end-of-lifetime criterion for O-ring seals under static conditions should include a safety margin for slight dimensional changes, a modified leakage test involving a small and rapid partial decompression of the seal was introduced that enabled determining a more realistic but still conservative end-of-lifetime criterion for an EPDM seal.
Both chain scission and crosslinking reactions occur during ageing of EPDM rubber. However, with many conventional polymer analysis methods such as hardness and DMA, it is hardly possible to obtain information about the contribution of each reaction type to the measured data. For example, hardness and Tg both increase during ageing of EPDM, indicating crosslinking during ageing, but it is not clear whether this is partly counterbalanced by chain scission reactions which would lower hardness and Tg. An indication that chain scission reactions probably counteract the hardness or Tg increase by crosslinking is given by Compression Set (CS) measurements. CS exhibits a higher change than hardness or Tg, as CS increases additively through both chain scission and crosslinking reactions. In order to elucidate the share of chain scission reactions in the total degradation, a method testing relaxation and recovery behaviour using DMA equipment was applied. The method revealed the strong influence of chain scissions, leading to more pronounced relaxation and higher residual strain after compression.
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.
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.
Thermoanalytische Charakterisierung von Ethylen-Vinylacetat-Copolymer (EVA) für Photovoltaikmodule
(2011)
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
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.