Size-controlled Synthesis of Gold Nanoparticles by Thermolysis of a Gold(I)-Sulfide Complex in the Presence of Alkylamines

A size-controlled synthesis of gold nanoparticles has been developed by the thermolysis of AuCl(SMe2) in the presence of alkylamines at 120 ◦C. In the procedure, the key intermediate was [Au(NH2R)2]Cl, detected by electrospray ionization (ESI) mass spectrometry. This thermally unstable intermediate was reduced by alkylamines under mild conditions to produce alkylamine-capped gold nanoparticles. The average diameters of the gold nanoparticles could be regulated in a range from 4.3 to 6.1 nm by applying primary alkylamines with alkyl chains of different lengths. Larger gold nanoparticles with diameters from 10 to 22 nm were prepared by a combination of alkylamines and alkylcarboxylic acids with various lengths of the alkyl chains. The gold nanoparticles were characterized by transmission electron microscopy (TEM), UV/Vis absorption spectroscopy, powder X-ray diffraction (PXRD), X-ray photoelectron spectroscopy (XPS), gas chromatography/mass spectroscopy (GC/MS), and thermogravimetric and differencial thermal analyses (TG/DTA).