We report on neutron transmutation doping (NTD) of isotopically (64Zn) enriched ZnO nanorods to produce material with holes as the majority mobile carrier. Nanorods of ZnO enriched with 64Zn were synthesised and the abundance of 64Zn in these samples is ∼ 71%, compared to the natural abundance of ∼ 49 %. The enriched material was irradiated with thermal neutrons which converts some 64Zn to 65Zn. The 65Zn decays to 65Cu with a half-life of 244 days and the Cu can act as an acceptor dopant. After 690 days, a hot probe technique was used to determine the majority charge carriers in non-irradiated and neutron irradiated nanorod samples. Non-irradiated samples were measured to be to have electrons as the majority mobile carrier and the irradiated samples were measured to have holes as the majority mobile carrier.