Tantalum(V) chloride was intercalated from the gas phase into highly oriented pyrolytic graphite and into natural graphite. Second stage intercalation compounds were produced. The TaCl5–graphite intercalation compounds were heated in a hydrogen atmosphere for 1week at 200°C. The flakes showed no exfoliation, but reduction was insufficient at this temperature. A reduction for 1week at 1000°C produced extensively exfoliated samples. After 1week at 1000°C in a hydrogen atmosphere, it was still possible to detect chlorine in some regions by energy-dispersive X-ray analysis. However, transmission electron microscope images showed the occurrence of nanometer-size particles within the graphite host lattice, located near the prismatic edges and also at the center of the particles. Different morphologies of the particles were observed, namely two-dimensional platelets and numerous one-dimensional `chains', with particle sizes between 10 and 300nm. Selected-area electron diffraction patterns of the particles gave evidence as to their chemical nature. Metallic tantalum was formed by the reaction, the patterns gave also evidence that a small amount of TaCl5 had still survived.