Seeing nanoscale electrocatalytic reactions at individual MoS₂ particles under an optical microscope: probing sub-mM oxygen reduction reaction

MoS₂ is a promising electrocatalytic material for replacing noble metals. Nanoelectrochemistry studies, such as using nanoelectrochemical cell confinement, have particularly helped in demonstrating the preferential electrocatalytic activity of MoS₂ edges. These findings have been accompanied by considerable research efforts to synthesize edge-abundant nanomaterials. However, to fully apprehend their electrocatalytic performance, at the single particle level, new instrumental developments are also needed. Here, we feature a highly sensitive refractive index based optical microscopy technique, namely interferometric scattering microscopy (iSCAT), for monitoring local electrochemistry at single MoS₂ petal-like sub-microparticles. This work focuses on the oxygen reduction reaction (ORR), which operates at low current densities and thus requires high-sensitivity imaging techniques. By employing a precipitation reaction to reveal the ORR activity and utilizing the high spatial resolution and contrast of iSCAT, we achieve the sensitivity required to evaluate the ORR activity at single MoS₂ particles.