This work presents a simple method to produce large quantities of crystallized antimony(0) nanoparticles through SbCl3 chemical reduction using t-BuONa-activated sodium hydride. t-BuONa acts as a superficial stabilizer of Sb(0) nanoparticles inhibiting their growth and avoiding aggregation. The Sb(O) nanoparticles were characterized using transmission electron microscopy, XPS analysis and X-ray powder diffraction. Results obtained show that rhombohedral Sb(0) with diameters of ca. 4.7 +/- 1.9 nm were produced. The influence of purification conditions on the aggregation state of Sb(O) particles is also described. (c) 2006 Elsevier B.V. All rights reserved.