A filament stretching rheometer for in situ X-ray experiments: Combining rheology and crystalline morphology characterization

We present a rheometer that combines the possibility to perform in situ X-ray experiments with a precise and locally controlled uniaxial extensional flow. It thus allows us to study the crystallization kinetics and morphology evolution combined with the rheological response to the applied flow field. A constant uniaxial deformation rate is ensured, thanks to a fast control scheme that drives the simultaneous movement of the top and bottom plates during a pulling experiment. A laser micrometer measures the time evolution of the smallest diameter, where the highest stress is concentrated. The rheometer has a copper temperature-controlled oven with the ability to reach 250 degrees C and a N-2 connection to create an inert atmosphere during the experiments. The innovation of our rheometer is the fixed location of the midfilament position, which is possible because of the simultaneous controlled movement of the two end plates. The copper oven has been constructed with four ad hoc windows: two glass windows for laser access and two Kapton windows for X-ray access. The key feature is the ability to perfectly align the midfilament of the sample to the laser micrometer and to the incoming X-ray beam in a synchrotron radiation facility, making it possible to investigate the structure and morphologies developed during extensional flow. The rheological response measured with our rheometer for low-density polyethylene (LDPE) is in agreement with the linear viscoelastic envelope and with the results obtained from the existing extensional rheometers. To demonstrate the capability of the instrument, we have performed in situ-resolved X-ray experiments on LDPE samples exhibiting extensional flow-induced crystallization.