Nickel microspheres were produced by the spark erosion technique under both liquid nitrogen and water conditions. Density measurements and Scanning electron microscope analysis revealed that a significant portion of the Ni particles produced under the liquid nitrogen conditions are hollow spheres with a density of 6.67(4)g/cm(3) while the particles produced in water are primarily solid spheres with a density of 8.40(1)g/cm(3), close to the bulk nickel value of 8.90 g/cm(3). Nickel/polymer composites incorporating the hollow and solid nickel microspheres were manufactured with volume fractions of 25% and 36%, respectively. The hollow and solid nickel composites exhibited saturation magnetostrictions of -24 and -28 ppm, respectively. In addition, small quantities of Terfenol-D (Tb0.3Dy0.7Fe2) were spark eroded under liquid argon conditions with similar to10% by volume of the spark eroded particles being solid microspheres. Calculations indicate that aligned composites that incorporate these Terfenol-D microspheres could reach a strain value of 2000 ppm.