A synthesis of new types of SbxOy/C composite negative electrodes for lithium and sodium-ion batteries is reported. Thin layers of graphitic carbon decorated in 3D with Sb nanoparticles were produced from organic precursors triphenylantimony (III) using a one-step microwave plasma chemical vapor deposition (MPCVD) method. Thin-film SbxOy/C electrodes were electrochemically tested in lithium and sodium half cells with Li and NaTDI (2-trifluoromethyl-4,5-dicyanoimidazole lithium and sodium salts) 0.75M electrolytes and delivered capacity of 425mAhg−1 at C/10 discharge rate.