Amorphous silicon oxycarbides are known to be an effective anode material for lithium‐ion batteries. Despite their exceptional properties and high charge capacities, however, their practical uses are limited by their significant first‐cycle loss, considerable hysteresis, and low cyclic ability. Comparatively, SiOC/metal oxide materials have demonstrated increased rate capability and cyclic stability. This study utilized a liquid precursor‐derived ceramic method to modify SiOC with titanium (IV) butoxide precursor to synthesize SiOC/TiOxCy. X‐ray diffractograms confirmed the amorphous nature of SiOC/TiOxCy. The elemental composition and bonding properties were investigated using X‐ray photoelectron spectroscopy, and electron microscopy was used to explore morphological features. In the first cycle, the reversible capacity of pyrolyzed SiOC/TiOxCy was 520 mAh g−1, which then increased to 736 mAh g−1 for the 1200°C annealed SiOC/TiOxCy due to the increased free carbon network and TiC conductive phases. The irreversible capacity of the first cycle was 568 mAh g−1, which was lower than the annealed SiOC irreversible capacity of 695 mAh g−1. Interestingly, the rate stability of the pyrolyzed SiOC/TiOxCy performed more stability than the annealed sample. Localized carbothermal reactions between amorphous SiOC/TiOxCy and free carbon at annealing temperatures resulted in loss of structure stability.
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