Synthesis and Photothermal Processing of Silicon‐Based Nanoconfined MXenes

Abstract Intercalation is a powerful approach to customize the properties of layered materials such as titanium carbide (Ti 3 C 2 T x ) MXenes. Photonic curing, a novel technique employing intense pulsed light from a xenon flashlamp (≈280–1100 nm wavelength range), offers significant advantages over conventional annealing methods. The pulsed nature of photonic curing enables rapid quenching, which allows trapping of metastable states and the formation of unique nanostructures. Herein, this work reports on the ion exchange intercalation of Ti 3 C 2 T x MXenes with aminopropyl terminated polydimethylsiloxane (amino‐PDMS) and the subsequent application of photonic curing to study pyrolysis of intercalated PDMS. The results showed an increase in the interlayer spacing ( d ‐spacing) of Ti 3 C 2 T x from 1 to 13.5 nm for the 5 kg mol −1 amino‐PDMS (5K‐PDMS) intercalant. After photonic curing, the intercalated PDMS is converted into SiO x or silicon oxycarbide, and the d ‐spacing decreased from 13.5 to 11 nm. Furthermore, curing the intercalated MXenes under controlled pressure in different gas environments, this work observes the conversion of PDMS to silicon carbide on the surface of MXenes layers. This study demonstrates the potential of photonic curing as a promising approach for cost‐effective, instantaneous, and scalable synthesis of customizable layered materials with precise control over the nanostructure within the layers.