Cathode materials are essential for enhancing electrocatalytic activity in energy-conversion devices. Carbon is one of the most suitable cathodic materials for Li–O2 batteries owing to its chemical and thermal stability. Carbon materials synthesized from tributyl borate (TBB) using a nonthermal solution plasma method were characterized using x‐ray diffraction, Raman, field emission scanning electron microscopy (FE-SEM), transmission electron microscopy, and x-ray photoelectron spectroscopy and were evaluated as additive materials for cathodes in a Li–O2 battery. Two separate carbon materials were formed at the same time, a carbon dispersed in solution and a carbon precipitate at the bottom of the reactor, which had amorphous and graphite-like structures, respectively. The amorphous carbon contained boron and tungsten carbide, and the graphite-like carbon had more defects and electronic conductivity. The crystallinity and density of defects in the graphite-like carbon could be tuned by changing the SP operating frequency. The Li–O2 battery with the amorphous carbon containing boron and tungsten carbide was found to have a high capacity, while the one with the graphite-like carbon showed an affinity for the formation of Li2O2, which is the desired discharge product, and exhibited high cycling performance.