Fe-Si-Zn alloys prepared by ball milling were investigated as negative electrodes for Li-ion batteries. X-ray diffraction and room temperature Fe-57 Mossbauer measurements were used to characterize alloy structure. Electrochemistry of the alloys was determined at 30 degrees C. Formation of crystalline Li15Si4 was suppressed during cycling for compositions with greater than 10 at. % Fe. Unlike sputtered films of the same composition, the incorporation of Zn in these ball milled alloys did not suppress Li15Si4 formation. Instead, Zn behaved as if it were in a physical mixture with the other alloy components. This study shows that sputtered and ball milled alloys of the same composition can have very different electrochemical properties. (C) 2015 The Electrochemical Society.