Here, we report the synthesis, characterization, and properties of Fe/Fe3O4 core shell nanocubes prepared via a simple route. It includes NaBH4 reduction of FeCl3 in an ethylene glycol solution in the presence of 2-mercaptopropionic acid (surfactant) and trisodium citrate (cosurfactant) followed by surface oxidation with trimethylamine N-oxide. The morphology and structure of Fe/Fe3O4 core shell nanocubes were characterized using transmission electron microscopy (TEM), high-resolution TEM, selected area electron diffraction, X-ray powder diffraction, and X-ray photoelectron spectroscopy. All of the methods confirm a Fe/Fe3O4 core shell structure of nanocubes. Magnetic measurements revealed that the Fe/Fe3O4 core/shell nanocubes are superparamagnetic at 300 K with a saturation magnetization of 129 emu/g. The T-2 weighted imaging and the T-2 relaxation time showed high MRI contrast and sensitivity, making these nanocubes viable candidates as enhanced MRI contrast agents.