Synthesis of supported metal nanoparticles (Au/tio₂) by the suspension impregnation method

This work reports a new technique called “Suspension Impregnation Method” (SiM) as an alternative to the “Incipient Impregnation Method” (IiM) for the synthesis of noble metal (Au) nanoparticles. The SiM was used to synthesize gold nanoparticles supported by titanium oxide and compared with those of IiM. The reactor for the SiM technique was based on the principles of mixing, heat, and mass transfer of the suspension reactors and the metal particle synthesis was processed in situ under the oxidation reduction potentials. Three different conditions were established to observe the effect of pH on the size of the metal particles: acid (HCl), neutral (water) and alkaline (urea). The samples were characterized by nitrogen adsorption, X-Ray Diffraction (XRD), Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES), Thermogravimetric Analysis (TGA)/Differential Thermal Analysis (DTA), Transmission Electron Microscopy (TEM) and CO₂ adsorption. The surface area was slightly modified, and the average pore diameter was reduced in all materials. The structure of the titanium oxide was not altered. A deposit of organic material was detected in samples synthesized in alkaline medium for both methods. The pH influenced the formation of conglomerates in IiM and resulted in large particle sizes (3–9 nm). In contrast, an in situ reduction in the species in SiM resulted in smaller particle sizes than IiM (2–3 nm).