Real-Time Multiscale Imaging of Heterogeneous Multistage Reactions: Insights into Nanoscale TiO Synthesis.

Hydrothermal methods are widely used to synthesize functional inorganic materials. The interplay between the reactive species, solution chemistry, and the nanoscale product makes it challenging to control the reaction pathway to achieve a uniform product. Here, we resolve the heterogeneity that arises during hydrothermal synthesis across different length scales.

Resolving Fast Relative Kinetics in Inorganic Solid-State Synthesis.

Solid-state syntheses are generally regarded as being slow, limited by transport, and, as such, are often only stopped to check the products after many hours at high temperature. Here, using a custom-designed reactor to rapidly initiate solid-state syntheses, we are able to capture the earliest stages of a reaction using X-ray scattering. For the reaction of TiO and LiCO to form spinel lithium titanate (LiTiO)─an anode material for fast-charging applications─we capture two distinct kinetic regimes, including fast initial kinetics in the first seconds-minutes of the reaction that account for significant product formation.