Publication date: 15th May 2025
Amphiphilic thiols perform dual roles in the synthesis of colloidal metal sulfide nanoparticles by ligating the particle surface and solubilizing precursor elements. The chemical processes involved in synthesis have important consequences for the yield and morphology of particles as well as their ligation, and these processes are not fully understood. In this study, we separate a typical synthetic procedure into a series of isolated physical experiments and characterize the products and byproducts of each reaction. Using in situ and ex situ absorption and photoluminescence spectroscopy and 1H NMR, we identify four key reactions: formation of metal thiolate, thermolysis yielding metal sulfide and thioether, thermolysis yielding hydrogen sulfide and alkene, and reaction of hydrogen sulfide with additional metal carboxylate. A window of solubility for thiolate-ligated particles is identified, the duration of which depends on the organic moiety of the thiol. The ability to modify surface functionality post-synthesis, exemplified by phase transfer to water, is found to depend on the native ligation, which depends on the yield of metal sulfide growth. The resistance of thiolate-ligated particles to subsequent exchange is further demonstrated in a novel technique for extracting differently-ligated particles from a homogeneous mixture.
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