Catalysts with Au and Pd supported on TiO2 (Au:Pd 1:1wt/wt%) were prepared by 1- and 2-nozzle flame spray pyrolysis (FSP). The 2-nozzle configuration allowed to synthesize various particle configurations by separate or co-feeding of the metal precursor solutions to the two nozzles. For the Au-Pd/TiO2 system, four different catalyst particle configurations were investigated: “TiO2+AuPd”, “Pd/TiO2 +Au”, “Au/TiO2 +Pd”, and “Pd/TiO2+Au/TiO2”, where+separates the corresponding precursor solutions fed to the two nozzles. There were no significant differences in the specific surface areas and the average TiO2 crystallite sizes of the catalysts (100m2/g and 16–17nm, respectively) with the exception of “Pd/TiO2 +Au/TiO2”, which exhibited larger surface area and smaller crystallite size (152m2/g, 12nm) due to halving of the Ti precursor concentration in each nozzle. As revealed by CO chemisorption, XPS, and STEM-EDX results, the catalyst properties varied largely in terms of bimetallic AuPd particle compositions, the interaction between metal–metal and metal-support, and the location of Pd (or AuPd) on the TiO2. Among the catalysts studied, “TiO2+AuPd” prepared with the 2-nozzle system exhibited the highest conversion of acetylene (∼50%) at 40°C with high selectivity to ethylene (>95%). Co-feeding the noble metal precursors together with the Ti precursor afforded less active catalysts due to the formation of Ti-O species partially covering the most active bimetallic AuPd particles. Compared to the commercially available acetylene hydrogenation catalyst and the AuPd/TiO2 prepared by conventional co-impregnation and deposition-precipitation, all the FSP-AuPd/TiO2 catalysts showed superior performances under the reaction conditions used.