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We present the effect of oxidative etching in FLG/TiO$_2$ hybrids on FLG edges chemistry/morphology addressing also the catalytic activity of TiO$_2$ NPs. According to the XPS and TGA analysis the oxidation degree strongly depends on TiO$_2$:FLG ratio. The preparation of two series of FLG/TiO$_2$ hybrids via sol-gel method and in-situ oxidation permitted to correctly describe and distinguish the chemical composition, core shift and charge distribution in C1s XPS with Tip peak as reference. Such analysis is challenging in carbon materials due the overlapping of C1s peaks from the sample and adventitious carbon reference. We claim the formation of interfacial dipole as possible direct signature of charge transfer from TiO$_2$ to FLG. A downward shift of C1s (sp$^2$C) up to 1.4 eV is measured and contributions of non sp$^2$C are determined in the composites. The modifications related to the oxidation are supported by TEM/SEM observations, and referred to non-catalytic oxidation and oxidation in mechanically mixed components. KEYWORDS: oxidative etching, graphene edges, TiO$_2$ catalyst, interfacial dipole, XPS, charge transfer

Four series of PLA based composite films containing horizontally aligned few layer graphene (FLG) flakes of high aspect ratio and adsorbed albumin are prepared. The mechanical and thermal properties vary with percentage, dispersion degree and size of FLG flakes. Great improvement up to 290 and 360% of tensile modulus and strength respectively was obtained for the composite containing high lateral size of FLG at 0.17% wt., and up to 60 and 80% for the composite with very well dispersed 0.02% wt. FLG. The composites of PLA and PEG-PLLA containing very well dispersed FLG flakes at 0.07 % wt. are ductile showing enhancement of elongation at break up to respectively 80 and 88%. Relatively high electrical conductivity, 5 x 10-3 S/cm, is measured for PLA film charged with 3% of FLG.

Quasi all water soluble composites use graphene oxide (GO) or reduced graphene oxide (rGO) as graphene based additives despite the long and harsh conditions required for their preparation. Herein, polyvinyl alcohol (PVA) films containing few layer graphene (FLG) are prepared by the co-mixing of aqueous colloids and casting, where the FLG colloid is first obtained via an effcient, rapid, simple, and bio-compatible exfoliation method providing access to relatively large FLG flakes. The enhanced mechanical, electrical conductivity, and O2 barrier properties of the films are investigated and discussed together with the structure of the films. In four different series of the composites, the best Young modulus is measured for the films containing around 1% of FLG. The most significant enhancement is obtained for the series with the largest FLG sheets contrary to the elongation at break which is well improved for the series with the lowest FLG sheets. Relatively high one-side electrical conductivity and low percolation threshold are achieved when compared to GO(rGO) composites (almost 10-3 S.cm-1 for 3% of FLG and transport at 0.5% FLG), while the conductivity is affected by the formation of a macroscopic branched FLG network. The composites demonstrate a reduction of O2 transmission rate up to 60%.