A simple procedure has been developed to prepare thiol-derivatized nanoparticles of metals. The procedure involves the transfer of well-characterized metal hydrosols to a hydrocarbon medium containing the thiol. Thiol-derivatized nanoparticles Au, Ag, and Pt of near spherical shape forming nanocrystalline arrays have been characterized by X-ray diffraction, transmission electron microscopy (TEM), and other techniques. Thiolderivatized Au particles of mean diameters of 1.0, 2.1, and 4.2 nm from nanocrystalline arrays show characteristic X-ray diffraction patterns. The nanoparticles exhibit Moiré fringes when deposited on a flake of MoSe 2 , showing that each particle is in itself crystalline. Besides spherical nanoparticles, thiol-derivatized particles of other shapes have been prepared, hexagonal Pt nanoparticles being particularly novel. Scanning tunneling microscopy images not only confirm the size and shape of nanoparticles revealed by TEM, but also show evidence for thiol molecules on the surface.

A new, facile and generally applicable synthesis of functionalized gold nanoparticles is presented. It is based on the surfactant-free generation of weakly stabilized nanoparticles by the reduction of HAuCl4 with sodium naphthalenide in diglyme. These nanoparticles were found to lack long-term stability. However, stabilization in both unpolar and polar solvents could straightforwardly be achieved by subsequent addition of various capping ligands. The resulting ligand-capped gold nanoparticles were investigated by TEM microscopy, UV-vis, and FT-IR spectroscopy. Particle core size can be tuned by the amount of reduction agent. The strict separation of the reduction step and the functionalization step in this one-pot synthesis offers an easy and fast access to highly functionalized gold nanoparticles.

Noble metal powders (Au, Ag, Pt, Pd and Ru) have been synthesized by the polyol process in both the nanometer and submicron scales (sans Pd, Pt and Ru). They have been characterized by both microscopic (TEM and SEM) as well as spectroscopic techniques (FT-IR and XPS). Infrared spectroscopy was employed to study the colloid particles in the presence of ethylene glycol and PVP and the results show that the interaction between the organic phase and the metal particles vary according to the particle size. The role of the solvent, ethylene glycol, during the reduction process was also investigated and we observe formation of >C=O vibration band after the reduction process implying that the solvent reduces the metal ions thereby getting oxidized. XPS measurements carried out on the colloidal sols have shown the presence of the organic phase adsorbed onto the metal particles.

Superlattices formed by arrays of Pt or Au nanoparticles have been obtained by layer-by-layer deposition by using dithiols as cross-linkers. The superlattices have been characterized by X-ray diffraction, photoelectron spectroscopy, and scanning tunneling microscopy. The core-level intensities of the metal and of the dithiol in the X-ray photoelectron spectra show the expected increase with successive depositions. The formation of such structures has been confirmed by depositing Pt and Au layers alternatively. Layers of metal and CdS nanoparticles have been deposited alternatively to obtain heterostructures.

Fig. 3 TEM images of thiol-derivatised Pt (a) and Ag (b) nanoparticles 538