© 2017 American Chemical Society. Thermal decomposition is a promising route for the synthesis of highly monodisperse magnetite nanoparticles. However, the apparent simplicity of the synthesis is counterbalanced by the complex interplay of the reagents with the reaction variables that determine the final particle size and dispersity. Here, we present a combined experimental and theoretical study on the influence of the heating rate on crystal growth, size, and monodispersity of iron oxide nanoparticles. We synthesized monodisperse nanoparticles with sizes varying from 6.3 to 27 nm simply by controlling the heating rate of the reaction. The nanoparticles show size-dependent superparamagnetic behavior. Using numerical calculations based on the classical nucleation theory and growth model, we identified the relative time scales associated with the heating rate and precursor-to-monomer (growth species) conversion rate as a decisive factor influencing the final size and dispersity of the nanoparticles.