The curvature-based technique is widely used to monitor stresses in thin film-substrate structures. The fundamental theory is based on the Stoney formula and its extensions, which mostly represents the average stress in thin films. However, the characterization of incremental stresses has not been clearly described, which leads to significant limitations in its application scope. Here, a formula for the incremental stress of thin films is proposed by discretizing the film growth layer for use in arbitrary modulus and thickness ratios. In specific cases, this formula can be manifested as Stoney's and Freund's formulas. The stress of electrodeposited Ni with different current densities was measured in situ for substrates at different elastic moduli and thicknesses. The formula was proven to be a more accurate expression of the incremental stress compared with averaging using Freund's formula or from the slope method. Furthermore, the proposed formula can be applied to arbitrary modulus and thickness ratios. This method provides valuable insight to monitor stresses in thin films and paves the way for further understanding the mechanisms of stress generation.
In recent years, the demand for polymer compound solutions for the application of bipolar plates in polymer electrolyte membrane fuel cells (PEMFC) has increased continuously due to significant cost and lifetime advantages compared to metallic solutions. The main challenge of the compounds is the high filler content required to ensure sufficient electrical conductivity of the bipolar plates. The associated increase in viscosity and simultaneously increased thermal conductivity limit the conventional injection molding process in terms of achievable flow path length to wall thickness ratios (plate aspect ratio). In order to evaluate the extent to which highly modified electrically conductive polymer material systems can be processed into thin-walled and highly dimensionally stable bipolar plates, an injection compression molding process with dynamic mold temperature control (ICM-DT) has been developed. For this purpose, a compound was prepared from polypropylene (PP) and graphite-flakes. The compound was characterized with respect to the achieved filler content, the electrical conductivity, as well as the pressure- and temperature-dependent solidification range. The ICM-DT experiments were carried out by varying the maximum mold temperature and the compression force. In addition, the process was designed with multiple compression and decompression steps to account for a possible pressure-dependent solidification of the compound. The plates were characterized with respect to the achieved plate aspect ratio and the flow-path-dependent dimensional thickness stability. It was shown that the plate aspect ratio could be increased by up to 125% with the maximum filler content compared to conventional injection molding processes provided in the literature. With the multi-stage ICM-DT process, it was also possible to optimize the thickness dimensional stability with a maximum deviation of 3% over the flow path.
The demand for polymer composite solutions in bipolar plates for polymer electrolyte membrane fuel cells (PEMFCs) has risen due to advantages over metal plates such as longer lifetime, weight reduction, corrosion resistance, flexible manufacturing, freedom of design, and cost-effectiveness. The challenge with polymer composites is achieving both sufficient electrical conductivity and mechanical stability with high filler content. A carbon fiber fleece as reinforcement in a graphite-filled polypropylene (PP) matrix was investigated for use as bipolar plate material with increased mechanical and sufficient conductive properties. Plates with a thickness of 1 mm containing four layers of fleece impregnated in the PP-graphite compound were produced in a compression molding process. Particle and fiber interactions were investigated via microscopy. The plates were characterized with respect to the electrical conductivity and mechanical stability. High electric conductivity was reached for fiber-reinforced and plain PP-graphite compound plates, with increased filler content leading to a higher conductivity. The contact resistance remained largely unaffected by surface etching as no polymeric skin layer formed during compression molding. Fiber-reinforced plates exhibit twice the tensile strength, a significantly higher tensile modulus, and an increased elongation at break, compared to PP filled only with graphite.
This study presents a method for the determination of the dynamic pressure-dependent solidification of polycarbonate (PC) during flow using high pressure capillary rheometer (HPC) measurements. In addition, the pressure-dependent solidification was determined by isothermal pressure-volume-temperature (pvT) measurements under static conditions without shear. Independent of the compression velocity, a linear increase of the solidification pressure with temperature could be determined. Furthermore, the results indicate that the relaxation time at a constant temperature and compression rate can increase to such an extent that the material can no longer follow within the time scale specified by the compression rate. Consequently, the flow through the capillary stops at a specific pressure, with higher compression rates resulting in lower solidification pressures. Consequently, in regard to HPC measurements, it could be shown that the evaluation of the pressure via a pressure hole can lead to measurement errors in the limit range. Since the filling process in injection molding usually takes place under such transient conditions, the results are likely to be relevant for modelling the flow processes of thin-walled and microstructures with high aspect ratios.
Integrative simulation techniques for predicting component properties, based on the conditions during processing, are becoming increasingly important. The calculation of orientations in injection molding, which, in addition to mechanical and optical properties, also affect the thermal shrinkage behavior, are modeled on the basis of measurements that cannot take into account the pressure driven flow processes, which cause the orientations during the holding pressure phase. Previous investigations with a high-pressure capillary rheometer (HPC) and closed counter pressure chamber (CPC) showed the significant effect of a dynamically applied pressure on the flow behavior, depending on the temperature and the underlying compression rate. At a constant compression rate, an effective pressure difference between the measuring chamber and the CPC was observed, which resulted in a stop of flow through the capillary referred to as dynamic compression induced solidification. In order to extend the material understanding to the moment after dynamic solidification, an equilibrium time, which is needed until the pressure signals equalize, was evaluated and investigated in terms of a pressure, temperature and a possible compression rate dependency in this study. The findings show an exponential increase of the determined equilibrium time as a function of the holding pressure level and a decrease of the equilibrium time with increasing temperature. In case of supercritical compression in the area of a dynamic solidification, a compression rate dependency of the determined equilibrium times is also found. The measurement results show a temperature-invariant behavior, which allows the derivation of a master curve, according to the superposition principle, to calculate the pressure equilibrium time as a function of the holding pressure and the temperature.