Blended elemental W–7 wt.%Ni–3 wt. %Fe powders were mechanically alloyed in a planetary ball mill and a heavy duty attritor. The structural and morphological characteristics of the as-milled powders were characterized by x-ray diffraction and electron microscopy techniques. A ternary solid solution of Fe and Ni in W formed in both the cases; the amount of Ni and Fe dissolved is higher in the attritor-milled powder than in the ball-milled powder. Morphologically, the W-rich particles in the attritor-milled powders were spheroidal, smaller in size, and showed a narrower size distribution than in the ball-milled condition. These differences led to increased density in the attritor-milled powder compact and significant differences in chemical composition of the matrix region and W-rich grains. Transmission electron microscopy investigations of the matrix region in the compacts revealed the presence of Fe2W precipitates uniformly distributed in an Ni(Fe, W) matrix.