Nanocomposites containing silicon and titanium nitride were synthesized by high-energy mechanical milling. The process results in very fine Si particles distributed homogeneously inside the TiN matrix. Si/TiN nanocomposites synthesized using different experimental conditions were evaluated for their electrochemical properties. Results indicate that Si in the composite alloys and dealloys with lithium during cycling, while TiN remains inactive providing structural stability. A composite containing 33.3 mol % Si obtained after 12 h milling exhibited a stable capacity of similar to 300 mAh/g, suggesting its promising nature. Preliminary cycling data show good capacity retention reflective of good phase and microstructural stability as verified by X-ray diffraction and scanning electron microscopy analyses.