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Nanocomposites of equimolar enantiomeric polylactide blends with multiwall carbon nanotubes (MWCNTs) were prepared by a solvent casting/sonication procedure. The first objective of the study was to investigate the effect of MWCNTs as nucleating agents for the selective crystallization of the polylactide (PLA) stereocomplex to obtain PLA‐based nanocomposites. Transmission Electron Microscopy (TEM) studies revealed large agglomerates and poor distribution of the non‐functionalized MWCNTs within the matrix. To enhance the compatibility between PLA and MWCNTs, pyrene‐end‐functionalized PLLA (py‐end‐PLLA) nanocomposites were prepared because of the ability of the pyrene moieties to interact with the MWCNTs via π−π stacking, and were subsequently blended with poly(d‐lactide) (PDLA) to investigate the possibility of achieving nanocomposites in which the enantiomeric blend crystallizes as stereocomplex. The resulting nanocomposites were characterized by Differential Scanning Calorimetry (DSC), X‐ray Diffraction (XRD), TEM, and Nuclear Magnetic Resonance Spectroscopy (NMR), revealing that MWCNTs were efficient nucleating agents for the overall crystallization of the blends. Interestingly, full stereocomplexation could be achieved with the aid of soft specific thermal treatments. According to these results, the addition of small amounts of MWCNTs combined with a mild thermal treatment might extend the processing window for the preparation of polylactides exclusively crystallized in the stereocomplex form. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 130: 4327–4337, 2013

Ultrasound micro-molding technology was successfully applied to prepare nanocomposites based on a poly(ε-caprolactone) (PCL) matrix and multi-walled carbon nanotubes (MWCNTs). Optimization of processing parameters (i.e., amplitude, force and time) was crucial to obtain nanocomposites without any evidence of degradation, high material saving and short processing time (7-8 s). Good dispersion of nanotubes was achieved after processing previously formed solvent casting films. This dispersion was even partially detected in pieces directly obtained from powder mixtures of both components. Incorporation of MWCNTs had a remarkable influence on melting and crystallization processes, which were systematically studied by time resolved synchrotron experiments. Results indicated higher melting and crystallization temperatures for the nanocomposite, with temperature differences higher than 5 • C. Carbon nanotubes were effective nucleating agents and had an influence on crystallinity, crystallization rate and even on lamellar morphology, which was evaluated by analysis of the correlation function of small angle diffraction profiles. Crystallinity within lamellar stacks was lower for the solvent casting nanocomposite, but in this case lamellae underwent a thickening process during heating that accounted for the increase in the melting temperature. Crystallization from the melt rendered similar lamellar morphologies at the end of the process due to a lamellar insertion mechanism.