An in-situ TEM microreactor for real-time nanomorphology & physicochemical parameters interrelated characterization

Abstract In-situ quantitative structure-property relationship (QSPR) characterization between nanomorphology and physicochemical parameters is essential for revealing the growth mechanism and guiding the optimization of functional nanomaterials. However, extracting the interrelated physicochemical parameters in the process of nanomorphology observation is still challenging. Herein, this paper demonstrates an advanced chip-scale platform for in-situ QSPR characterization by integrating a gravimetric resonant microcantilever sensor within a transmission electron microscopy (TEM) microreactor. The microcantilever measures the thermodynamic and kinetic parameters, such as enthalpy (ΔH°), activation energy (Ea) and reaction rate (v), by monitoring the reaction-induced mass change of functional nanomaterials. Simultaneously, the low-stress SiNx films as electron transparent windows allow in-situ nanomorphology observation. Using such a QSPR characterization platform, the three-stage sulfuration mechanism based on nano Kirkendall effect for the gas-solid reaction of H2S and Cu nanowires is revealed, and the different molecule-interaction behaviors of SO2 on ZnO nanowires at various temperatures are distinguished for the first time. It is believed that the in-situ QSPR microreactor can be widely used for elucidating the underlying interfacial thermodynamic/kinetic reaction mechanism, and guiding the controllable synthesis and precise optimization of functional nanomaterials.