Single crystals of the spin dimer compound Pb2V3O9 were grown for the first time by the floating zone method. Room temperature single-crystal X-ray diffraction measurements confirm their crystallinity and structure. The crystal growth process is discussed in detail and high temperature differential scanning calorimetry measurements that show a structural phase transition from a monoclinic to a triclinic unit cell at 759(1)K are presented. Published by Elsevier B.V.