We present a high-scale method to produce few-layer graphene (FLG) based on the mechanical exfoliation of graphite and compare the obtained FLG with the one reported earlier arising from pencil lead ablation. Several elements were modified and improved in the new approach. The purification and the ablation set-up were simplified, and the morphology of the FLG was modified and improved in view of some applications. The morphology-dependent properties of FLGs, lead-FLG, and graphite-FLG as conductive layers and in nanocomposites were investigated. The newly obtained FLG had a higher aspect ratio (high lateral size vs thickness/higher 2D aspect), which is reflected by enhanced transparency–conductivity features of the layer (film) and elongation-at-break behavior of the polymer composites. On the contrary, the nanocomposite containing lead-FLG showed, for instance, excellent gas barrier properties due to the multi-step structure of the lead-FLG flakes. Such structure exhibited less 2D and more 3D character, which can be highly suitable for applications where the presence of active/reactive edges is beneficial, e.g., in catalysis or supercapacitors’ electrodes. Nuclear reaction analysis was employed to investigate the morphology of graphite-FLG film.
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