Polymer research and synchrotron radiation perspectives
A 5-minute read
This paper shows how synchrotron radiation-based polymer research has advanced significantly over the past 20 years. This has made it possible to study materials outside of equilibrium settings as well as in conditions that start to roughly resemble realistic processing conditions, which has greatly increased the level of experimental sophistication.
Figure 1. Derived parameters from a SAXS/WAXS/DSC/calometric/conductivity experiment obtained during thermal treatments of a polymer sample doped with Multi Walled Carbon Nano Tubes. (A) Thermal profile, (B) raw data, (C ) derived electron density data (SAXS), (D) Raw WAXS data, (E) degree of crystallinity derived from WAXS data, (F) thermal diffusivity, (G) electrical conductivity. Data obtained with modern detectors and sample environments.
Both WAXS or SAXS studies could be used to follow the kinetics of crystallization with a respectable degree of accuracy. In the case of WAXS, one could take the peak intensities and observe how these developed from the disordered melt. Meanwhile, by employing SAXS one may track the rise in electron density and utilize it as a gauge for the rise in crystallinity level. One of the most important steps in this study was the introduction of combined SAXS/WAXS experiments. This enabled for the first time to observe the events taking place at the different length scales that were involved.
Data quality is improved as shown in Fig. 1. This shows results from a combined SAXS/WAXS/DSC/conductivity experiment on poly(epsilon-caprolactone) to which multiwalled carbon nanotubes were added in order to form a nanocomposite. In calorimetric tests, two melting peaks with various characteristic temperatures were discovered for PCL/MWCNT composites, whereas pure PCL only exhibits one melting peak. Pure PCL heterogeneities serve as the heterogeneous nuclei that cause crystallization to begin upon cooling at a rate of 10 K/min. The melting peak at higher temperatures is related to crystals epitactically formed from MWCNT surfaces at higher temperatures. In comparison to the heterogeneities in the plain polymer, the MWCNTs are more effective heterogeneous nuclei.
Reference
[1] Wurm, A., Lellinger, D., Minakov, AA, Skipa, T., Pötschke, P., Nicula, R., Alig, I., & Schick, C. (2014). Crystallization of poly( ε-caprolactone)/MWCNT composites: A combined SAXS/WAXS, electrical and thermal conductivity study. Polymer , 55 (9), 2220–2232. https://doi.org/10.1016/j.polymer.2014.02.069