In this paper, a novel method for the double heat treatment of ductile iron was applied. Ten sets of specimens (three specimens in each set) of ductile cast iron (DCI) containing 0.51% wt. Cu were prepared and converted to austenitic ductile iron. All specimens were austenitized at 850 °C for 60 min and annealed at 420 °C, 331 °C and 250 °C for 120, 68 and 30 min, respectively. Five sets of samples were then annealed at 500 °C for 60 min, creating a novel double heat treatment process for annealing. Finally, all specimens were slowly cooled in air at ambient temperature. Tensile strength, hardness and elongation were measured in all specimens to compare the specimens with and without subsequent tempering. A microstructural analysis was also performed, which showed that the microstructure changed for the specimens that were subsequently tempered with. The results show that specimens with subsequent tempering have slightly higher hardness, a small decrease in tensile strength and significantly higher elongation. In addition, specimens with subsequent tempering exhibit more uniform mechanical properties compared to specimens without subsequent tempering. The use of neutron beam techniques was proposed to further characterize the newly formed microstructure after subsequent tempering.