To assess the impact of graphite fillers on the thermal processing of graphite/poly(lactic acid) (PLA) composites, a series of the composite samples with different graphite of industrial grade as fillers was prepared by melt mixing. The average size of the graphite grains ranged between 100 µm and 6 µm. For comparative purposes, one of the carbon fillers was expandable graphite. Composites were examined by SEM, FTIR, and Raman spectroscopy. As revealed by thermogravimetric (TG) analyses, graphite filler slightly lowered the temperature of thermal decomposition of the PLA matrix. Differential scanning calorimetry (DSC) tests showed that the room temperature crystallinity of the polymer matrix is strongly affected by the graphite filler. The crystallinity of the composites determined from the second heating cycle reached values close to 50%, while these values are close to zero for the neat polymer. The addition of graphite to PLA caused a slight reduction in the oxidation induction time (OIT). The melt flow rate (MFR) of the graphite/PLA composites was lower than the original PLA due to an increase in flow resistance associated with the high crystallinity of the polymer matrix. Expandable graphite did not cause changes in the structure of the polymer matrix during thermal treatment. The crystallinity of the composite with this filler did not increase after first heating and was close to the neat PLA MFR value, which was extremely high due to the low crystallinity of the PLA matrix and delamination of the filler at elevated temperature.

In this work, we present the characterization and electrochemical performance of various ternary silicon oxycarbide/graphite/tin (SiOC/C/Sn) nanocomposites as anodes for lithium-ion batteries. In binary SiOC/Sn composites, tin nanoparticles may be produced in situ via carbothermal reduction of SnO₂ to metallic Sn, which consumes free carbon from the SiOC ceramic phase, thereby limiting the carbon content in the final ceramic nanocomposite. Therefore, to avoid drawbacks with carbon depletion, we used graphite as a substitute during the synthesis of precursors. The ternary composites were synthesized from liquid precursors and flake graphite using the ultrasound-assisted hydrosilylation method and pyrolysis at 1000 °C in an Ar atmosphere. The role of the graphitic component is to ensure good electric conductivity and the softness of the material, which are crucial for long term stability during alloying–dealloying processes. The presented approach allows us to increase the content of the tin precursor from 40 wt.% to 60 wt.% without losing the electrochemical stability of the final material. The charge/discharge capacity (at 372 mA g⁻¹ current rate) of the tailored SiOC/C/Sn composite is about 100 mAh g⁻¹ higher compared with that of the binary SiOC/Sn composite. The ternary composites, however, are more sensitive to high current rates (above 372 mA g⁻¹) compared to the binary one because of the presence of graphitic carbon.

The hydroxylated carbon nanotubes (CNTs-OH), due to their propensity to trap electrons, are considered in many applications. Despite many case studies, the effect of the electronic structure of the CNT-OH electrode on its oxidation properties has not received in-depth analysis. In the present study, we used Fe(CN)₆^3−/4− and Ru(NH₃)₆^3+/2+ as redox probes, which differ in charge. The CNT-OH and CNT electrodes used in the cyclic voltammetry were in the form of freestanding films. The concentration of holes in the CNTs-OH, estimated from the upshift of the Raman G-feature, was $2.9\times {10}^{13} {\mathrm{c}\mathrm{m}}^{-2}$. The standard rate constant of the heterogeneous electron transfer (HET) between Fe(CN)₆^3−/4− and the CNTs-OH electrode was $25.9\times {10}^{-4} \mathrm{c}\mathrm{m}·{\mathrm{s}}^{-1}$. The value was more than four times higher than the HET rate on the CNT electrode ($k_s=6.3\times {10}^{-4} \mathrm{c}\mathrm{m}·{\mathrm{s}}^{-1}$), which proves excellent boosting of the redox reaction by the holes. The opposite effect was observed for the Ru(NH₃)₆^3+/2+ redox couple. While the redox reaction rate constant at the CNT electrode was $1.4\times {10}^{-4} \mathrm{c}\mathrm{m}·{\mathrm{s}}^{-1}$, there was a significant suppression of the redox reaction at the CNT-OH electrode ($k_s<0.1\times {10}^{-4} \mathrm{c}\mathrm{m}·{\mathrm{s}}^{-1}$). Based on the DFT calculations and the Gerischer model, we find that the boosting of the HET from the reduced form of the redox couple to CNT-OH occurs when the reduced forms of the redox couples are negatively charged and the occupied reduced states are aligned with acceptor states of the nanotube electrode.

High filled polylactide/multiwall carbon nanotube composites were subjected to multiple extrusions using single-screw and twin-screw extruders. Samples of the processed composites were characterized by SEM, XRD, Raman, and FTIR spectroscopy. Thermal and rheological properties were investigated by DSC and MFR analyses. Subsequent extrusions resulted in decreased torque and process efficiency, which is a consequence of the viscosity reduction of PLA. Thermal and rheological properties of composites changed after each extrusion as well. As revealed by DSC analyses, cold crystallization temperature showed a tendency to decrease after each process, whereas cold crystallization enthalpy ΔHcc increased significantly. Melt flow rate, which is indicative of the polymer degradation, increased after each extrusion.

Twin-screw extrusion is a crucial method for the direct inserting of carbon micro- and nanomaterials into a polymer matrix using a dry procedure. The study aimed to determine the influence of the parameters of the twin-screw extruder plasticizing system on the dispersion homogeneity and distribution of graphite filler in the polylactide polymer matrix and overall quality of the composite. As a filler, a graphite micropowder with a 5 μm lateral size of platelets was used at concentration of 1 wt.%. Three configurations of screws with different mixing intensity and various types segments were considered in the extrusion experiments. Morphology and chemical structure of the obtained composites were examined using scanning electron microscopy (SEM), Fourier transform infrared spectroscopy – attenuated total reflectance (FTIR-ATR) and Raman spectroscopy. Differential scanning calorimetry (DSC) and melting flow rate measurements (MFR) were used to asses thermal and rheological properties of the composites. Samples of the polylactide/graphite composites were also subjected to mechanical tests. The results show that the selection of the mechanical parameters of twin-screw extruder plasticizing system plays a key role in the preparation of the homogeneous PLA/graphite composites. Incorrect selection of the screw geometry results in poor mixing quality and a significant deterioration of the mechanical and thermal properties of the composites. Optimised mixing and extrusion parameters can be the starting point for the design of efficient twin-screw extruder plasticizing system for fabrication of PLA composites with carbon nanotube and graphene fillers.