Practical approaches to the synthesis
of atomically precise metal
nanoclusters are in high demand as they provide the structural basis
for investigating nanomaterials’ structure–property
correlations with atomic precision. The Brust–Schiffrin method
has been widely used, while the essential reductive ligands (e.g.,
thiols) limit the application of this method for synthesizing metal
nanoclusters with specific frameworks and surface ligands. In this
work, we developed a photochemical route for synthesizing atomically
precise metal nanoclusters by applying disulfide, which is a widely
available, stable, and environmentally friendly sulfur source. This
method enables the construction of structurally diverse metal nanoclusters
and especially features the synthesis of PhS-protected metal nanoclusters
that were not easily achieved previously and the gram-scale synthesis.
A reduction–oxidation cascade mechanism has been revealed for
the photochemical route. This work is expected to open up new opportunities
for metal nanocluster synthesis and will contribute to the practical
applications of this kind of nanomaterial.