In Situ Small-Angle X-ray Scattering Studies on the Growth Mechanism of Anisotropic Platinum Nanoparticles

[Image: see text] Shape-controlled platinum nanoparticles exhibit extremely high oxygen reduction activity. Platinum nanoparticles were synthesized by the reduction of a platinum complex in the presence of a soft template formed by organic surfactants in oleylamine. The formation of platinum nanoparticles was investigated using in situ small-angle X-ray scattering experiments. Time-resolved measurements revealed that different particle shapes appeared during the reaction. After the nuclei were generated, they grew into anisotropic rod-shaped nanoparticles. The shape, size, number density, reaction yield, and specific surface area of the nanoparticles were successfully determined using small-angle X-ray scattering profiles. Anisotropic platinum nanoparticles appeared at a low reaction temperature (∼100 °C) after a short reaction time (∼30 min). The aspect ratio of these platinum nanoparticles was correlated with the local packing motifs of the surfactant molecules and their stability. Our findings suggest that the interfacial structure between the surfactant and platinum nuclei can be important as a controlling factor for tailoring the aspect ratio of platinum nanoparticles and further optimizing the fuel cell performance.