Dynamics of the nanocrystal structure and composition in growth solutions monitored by in situ lab-scale X-ray diffraction

In situ characterization of nanoparticle (NP) growth has become the state-of-the-art approach for studying their growth mechanisms; there is broad consensus on the reliability and precision of in situ characterization techniques compared to more traditional ex situ ones. Nonetheless, most of the currently available methods require the use of sophisticated setups such as synchrotron-based X-ray sources or an environmental liquid transmission electron microscopy (TEM) cell, which are expensive and not readily accessible. Herein, we suggest a new approach to study NP growth mechanisms: using a commercially available heating chamber for time-resolved X-ray diffraction (TR-XRD) measurements of NP growth in solution. We demonstrate how this lab-scale in situ XRD can be used to study NP growth mechanisms when complemented by standard ex situ techniques such as TEM and UV–vis spectroscopy. TR-XRD reveals the crystallographic phase and real-time evolution of NP size, shape, and composition. A detailed analysis allows determining the growth mechanism and measuring the alloying kinetics of multinary nanocrystals, demonstrated herein for a colloidal CdxZn1−xS system. This approach proves itself as a promising strategy for NP growth research and could be expanded to related fields that study dynamic changes as the formation and evolution of crystalline materials in solutions.