Following the Kinetics of Barium Titanate Nanocrystal Formation in Benzyl Alcohol Under Near‐Ambient Conditions

In complex chemical syntheses (e.g., coprecipitation reactions), nucleation, growth, and coarsening often occur concurrently, obscuring the individual processes. Improved knowledge of these processes will help to better understand and optimize the reaction protocol. Here, a form‐free and model independent approach, based on a combination of time‐resolved small/wide‐angle X‐ray scattering, is employed to elucidate the effect of reaction parameters (such as precursor concentration, reactant stoichiometry, and temperature) on the nucleation, crystallization, and growth phenomena during the formation of nanocrystalline barium titanate. The strength of this approach is that it relies solely on the total scattered intensity (i.e., scattering invariant) of the investigated system, and no prior knowledge is required. As such, it can be widely applied to other synthesis protocols and material's systems. Through the scattering invariant, it is found that the amorphous‐to‐crystalline transformation of barium titanate is predominantly determined by the total amount of water released from the gel‐like barium hydroxide octahydrate precursor, and three rate‐limiting regimes are established. As a result of this improved understanding of the effect of varying reaction conditions, elementary boundary conditions can be set up for a better control of the barium titanate nanocrystal synthesis.