The structural and electrical characteristics of Ni nanocrystals embedded in high-k HfO 2 have been studied. High-resolution transmission electron microscopy revealed the formation of tiny Ni nanocrystals, in the average diameter of ϳ8 nm size for the sample annealed at 1000°C for 5 min. Atomic force microscopy shows the deposition of uniform Ni nanocrystals on a HfO 2 layer. A good hysteresis memory window of ϳ2.1 V at sweeping gate voltage of Ϯ15 V was observed in optimized annealed samples. A maximum flatband voltage shift of 2.1 Ϯ 0.05 V was accomplished for the optimized sample. The retention and leakage current of the metal oxide semiconductor capacitors were also studied.Floating gate memory structures based on charge storage in discrete semiconductor and metal nanocrystals ͑NCs͒ have recently attracted renewed interest for their potential applications in nextgeneration flash memory devices. 1-14 Embedded NCs in the floating gate sandwiched between tunnel and control oxide layers are charged by direct-tunnel electrons from the channel to shift the device threshold.The downscaling of tunnel oxide thickness leads to reduction in operation voltage to attain faster programming and erasing speeds. Current efforts are focused on replacing conventional SiO 2 in the flash memory gate stack with high-dielectric-constant ͑high-k͒ materials 2,3,8,11,15,16 to remove the limitation of scaling trend in controlling the gate tunnel current for flash memory devices and to enhance retention performance. Most of the studies, including ours, have focused on the fabrication of metal-oxide-semiconductor ͑MOS͒ structures having semiconductor NCs. 5-8 Nevertheless, MOS-based memory devices fabricated with metal NCs, like Au, 9 Ni,[9][10][11] Ru, 12 W, 13 Pd, 14 RuO x , 17 TiN, 18 etc., are considered to be more advantageous for their higher density of states around the Fermi level, a wide range of available work function, stronger coupling with conduction channels, and smaller energy perturbation due to carrier confinement, 19-22 with the semiconductor counterpart. The use of metal NCs also makes it possible to use smaller operating voltages while obtaining better endurance characteristics and faster write/erase speeds with smaller fluctuations and interface states due to its high work function in comparison to its semiconductor counterpart. 19,20 Among other metals, nickel, which is attractive for complementary MOS technology as metal gate electrodes 21 and source drain engineered devices, 22 has not been fully explored for nonvolatile memories. Due to their high work function ͑ϳ4.9 eV͒, Ni NCs result in deep quantum wells for the trapping of charge carriers. Most of the work based on Ni NCs has been performed using conventional silicon dioxide as a tunneling barrier.In this article, we report the electrical characteristics of Ni NC MOS structures using HfO 2 as tunneling and control dielectrics. The effect of postdeposition annealing on memory and the structural, interfacial, and electrical properties of the floating gate memo...