Amorphous alloys are one of the most important catalytic materials and considered as a new generation of metallic catalysts. Mastery over the composition and/or morphology of amorphous alloy enables control of its properties and enhancement of its applications as catalyst. The aim of this chapter is to present the recent developments in the design-and fabrication of amorphous alloys through chemical reduction method with an emphasis on composition-and morphology control. The examples discussed in this review highlight the need to design and synthesis of amorphous alloy with controllable composition or morphology in order to promote catalytic performances. Perhaps more importantly, they also are of value for researchers in the area of heterogeneous catalysis to develop highlyefficient metallic catalysts.