Abstract
An innovative experimental approach to study the electrodeposition of small nanoparticles and the early stages of electrochemical nucleation and growth is presented. Carbon coated gold TEM grids are used as substrates for the electrodeposition of silver nanoparticles so that electrochemical data, FESEM, HAADF–STEM and HRTEM data can be acquired from the same sample without the need to remove the particles from the substrate. It is shown that the real distribution of nanoparticles cannot be resolved by FESEM whereas HAADF–STEM analysis confirms that a distribution of ‘small’ nanoparticles (d ≈ 1–2 nm) coexist with ‘large’ nanoparticles corresponding to a bimodal size distribution. Besides, particles grown under the same conditions have been found to present different structures such as monocrystals, polycrystals or aggregates of smaller particles.
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