Accelerated Catalyst Development via Kinetically Controlled Solid‐State Laser Synthesis and Automated Electrochemical Screening

Wet chemical methods are widely employed for nanoparticle synthesis. While offering a high degree of tunability, they often require surfactants, high-temperature processing, and large solvent volumes. Here, we present a rapid, ambient-condition laser-based synthesis method for supported metal nanoparticles, enabling precise control over particle size and distribution homogeneity, the critical parameters in catalytic performance. By tuning laser fluence through power and scanning speed, we systematically explore the crystallite size distribution of platinum, palladium, and iridium nanoparticles supported on carbon. To accommodate the potentially high-throughput nature of laser synthesis, X-ray diffraction (XRD) data are analyzed via automated Rietveld refinement, which provides fast, consistent, and quantitative insights into crystallite size and distribution, further validated by scanning transmission electron microscopy (STEM). Real-time thermal imaging reveals material-specific decomposition thresholds, correlating laser parameters with nanoparticle formation dynamics. Integration with an automated scanning flow cell inductively coupled plasma mass spectrometry (SFC-ICP-MS) platform demonstrates the method's compatibility with high-throughput electrochemical screening, exemplified by stability testing of platinum catalysts for the oxygen reduction reaction (ORR). This approach offers a scalable and generalizable route for rapid catalyst discovery across diverse materials systems.