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In this work, we study the impact of the preceramic precursor vinyltriethoxysilane (VTES) on the electrochemical performance of silicon oxycarbide (SiOC) glass/graphite composites. We apply an innovative approach based on high-power ultrasounds in order to obtain highly homogenous composites with a uniform distribution of small graphitic flakes. This procedure enhances gelation and drying of VTES-based preceramic polymer/graphite blends. The SiOC/graphite composites reveal stable capacities (up to 520 mAh g−1 after 270 cycles), which are much higher than the sum derived from the ratio of the components. Additionally, the first cycle Coulombic efficiencies obtained for the composites are 15% higher than that of the pristine VTES-based SiOC ceramic. These properties are identified as the synergistic effect, originated from the addition of graphite to VTES-based SiOCs. Interestingly, such improvement in electrochemical performance is not noticed in the case of analogous SiOC/graphite composites based on phenyltriethoxysilane (PhTES) precursor. The microstructural investigation of the composites based on two different preceramic precursors using solid-state 29Si NMR and Raman Spectroscopy unveils the reason for such discrepancy in their electrochemical behaviour.