A microstructure study of colloidal gold nanoparticles by X-ray diffraction line profile analysis

We present the colloidal synthesis of gold nanoparticles (Au NPs) using the chemical reduction of gold precursors by changing the reducing agent (Na3C6H5O7) volume. We aimed at achieving different particle sizes, morphologies, and defect structures. The modified process impacted the overall synthesis time and nanoparticles' microstructures. We used X-ray diffraction profile analysis (XPA) and transmission electron microscopy (TEM) to follow the nanoparticles’ size and lattice strain details. The NPs' size distributions agree well between the indirect XPA and TEM direct measures. Nanocrystal shapes change from triangular, octahedral, and decahedral to hexagonal plate-like; it shows how the NPs minimize their energy formation by creating defects and well-defined crystallographic directions, including crystal fusion. The combined effects of dislocations, twin boundaries, and surface tension add together to broaden the diffracted line profiles. In particular, the density of dislocation and twin boundaries increase toward the smaller NPs.