The reduction of yttrium fluoride (YF 3 ) by calcium in a molybdenum crucible was investigated. A visual observation technique was used to monitor the reduction process. It was observed that the reaction initiated immediately after the melting of calcium. Based on the results, a two-step reduction sequence was attempted. First, the charge was heated to 9508C to minimise the calcium loss by vaporisation and to ensure completion of reaction. The products were then fast heated to 16008C for slag/metal separation. Molybdenum content of yttrium was found to be in a range of 3.5-4.75 wt-%, which is much lower than the equilibrium content predicted by Mo-Y phase diagram. The yttrium/molybdenum interface was studied using an electron probe microanalyser, which confirmed that the overall equilibrium was not reached, indicating the possibility of lowering the molybdenum contamination further by process optimisation.