0000000000033346
AUTHOR
Zebene Kiflie
Physical Cross Links in Amorphous PET, Influence of Cooling Rate and Ageing
A Continuous Cooling Transformation (CCT) procedure can be used to distinguish the initial “state” of the amorphous PET samples produced upon solidification from the melt at different cooling rates. The material frozen at this stage behaves as a rubber when brought above the Tg due to the onset of physical cross links. The rubber is not a stable network, however, since physical cross links may eventually dissolve. Their size distribution, and possibly their number, depend on cooling rate and ageing. Some may be even stable above the glass transition and act as nuclei for further crystallization from the glass. Upon increasing cooling rate, size distribution becomes smaller and stability of …
Linking structure and nanomechanical properties via instrumented nanoindentations on well-defined and fine-tuned morphology poly(ethylene)
Several poly(ethylene) samples with a broad range of morphologies were studied in this work using nanoindentations. The samples had degrees of crystallinity ranging from 30 to 100% while their Young's modulus ranged from few tens of MPa up to several GPa. Experimental conditions for the correct evaluation of Young's modulus were at first identified, choosing a suitable loading rate in order to minimize viscoelastic effects on the unloading. The force curves, i.e., plots of applied load vs. penetration depth, were then analyzed following two common procedures available in the literature. None of these procedures leads to satisfying results when compared to other experimental techniques. Howe…
Viscoelastic recovery behavior following Atomic Force Microscope nanoindentation of semi-crystalline poly(ethylene)
The residual imprint left behind by the AFM nanoindentation of polymers has been seldom studied in the past. In this work, the evolution of indentations at room temperature performed on a semicrystalline poly- (ethylene) in a broad range of experimental conditions is presented. The study shows that the recovery after 24 h is substantial, although not complete. Moreover, the dynamics of the recovery process is not seen to depend on the magnitude of the applied load for the nanoindentation, but instead on the rate of the indentation used. This points out that viscoelastic processes are minimized when performing fast nanoindentations, while at low loading rates there seems to be a residual vis…
The continuous cooling transformation (CCT) as a flexible tool to investigate polymer crystallization under processing conditions
An experimental route for investigating polymer crystallization over a wide range of cooling rates (from 0.01 to 1000◦C/s) and pressures (from 0.1 to 40 MPa) is illustrated, using a method that recalls the approach adopted in metallurgy for studying structure development in metals. Two types of experimental setup were used, namely an apparatus for fast cooling of thin films (100–200 μm thick) at various cooling rates under atmospheric pressure and a device (based on a on-purpose modified injection molding machine) for quenching massive samples (about 1–2 cm3) under hydrostatic pressure fields. In both cases, ex situ characterization experiments were carried out to probe the resulting struct…
Nanoscale mechanical characterization of polymers by atomic force microscopy (AFM) nanoindentations: viscoelastic characterization of a model material
The atomic force microscope (AFM), apart from its conventional use as a microscope, is also used for the characterization of the local mechanical properties of polymers. In fact, the elastic characterization of purely elastic materials using this instrument can be considered as a well-assessed technique while the characterization of the viscoelastic mechanical properties remains the challenge. In particular, one finds the mechanical behavior changing when performing indentations at different loading rates, i.e. on different time scales. Moreover, this apparent viscoelastic behavior can also be due to complex contact mechanics phenomena, with the onset of plasticity and long-term viscoelasti…
Role of thermal history on quiescent cold crystallization of PET
8 pags., 9 figs.
Non-isothermal crystallization kinetics of PET
The crystallization kinetics of poly(ethylene terephthalate) was studied using constant cooling rate, isothermal and quenching experiments. A non-isothermal crystallization kinetics equation based on a single mechanism was used to analyze the data. Different mechanisms of crystallization at low, intermediate, and high cooling rates were hypothesized based on deviation of the experimental data from the single mechanism model.
Mechanical properties of the nanometer scale pre-crystalline order of a poly (ethylene terepthalate) / poly (ethylene naphthalene) blend
A previous study carried out on PET has shown that this polymer undergoes a continuous structural modification over a wide cooling rate interval when solidified from the melt[1] assuming a semi-crystalline structure below 2 K s 1 and a completely amorphous one above 100 K s 1. Most important was the existence of a state of intermediate order between the above cooling rates which was evidenced by the absence of crystalline reflections in the WAXS patterns and the occurrence of SAXS maxima[2] and exothermic peak areas (DSC) in the cooling rate range above 2 K s 1. Microhardness (MH) measurements revealed that this phase affects the mechanical properties[3] plausible if one thinks of crystalli…