Single crystals of niobium substituted ~Fe203 were grown by using chemical vapor transport with tellurium tetrachloride and were characterized by using bulk methods (x-rays , resistivity, magnetism) and surface techniques (LEED, Auger, XPS). Niobium substituted ~Fe203 crystallizes with the corundum structure, and is an extrinsic n-type semiconductor with a room temperature resistivity of approximately 8SQcm, and an activation energy for conduct ivity of 0.22eV. Low temperature susceptibility measurements suggest that the substitution of niobium(V) in octahedral sites leads to reduction of iron (III) to iron(II) without ,spinel phase inclusions. The main face of the single crystal platelets is the (001) basal plane of a-Fe203.The surface is very well ordered as shown by LEED. These crystals show good potential for application in both photoelectrochemistry and surface science studies.