Silver nanoparticle solution was prepared by the addition of silver nitrate (AgNO 3 ), trisodium citrate dihydrate (C 6 H 5 Na 3 O 7 ·2H 2 O), sodium borohydride (NaBH 4 ), cetyltrimethyl ammonium bromide ((C 16 H 33 )N(CH 3 ) 3 Br), and ascorbic acid (C 6 H 8 O 6 ), which was subsequently added to distilled water. The resulting solution was subjected to ultrasonic irradiation for 3 h. [C 60 ]fullerene nanowhisker-silver nanoparticle composites were prepared using C 60 -saturated toluene, silver nanoparticle solution, and isopropyl alcohol by the liquid-liquid interfacial precipitation (LLIP) method. The product of [C 60 ]fullerene nanowhisker-silver nanoparticle composites was con rmed by x-ray diffraction, Raman spectroscopy, scanning electron microscopy, and transmission electron microscopy. The activity of [C 60 ]fullerene nanowhisker-silver nanoparticle composites as a catalyst was characterized by the reduction of 4-nitrophenol by UV-vis spectroscopy.