The large surface, the excellent dispersion and the high degrees of sensitivity of bimetallic nanocatalysts are the attractive features of this investigation. Carbon materials have special electronic properties and are considered promising materials for batteries, biosensors, fuel cells, and optically transparent electrodes. Graphene foam (GF) is a three dimensional (3D) porous architecture consisting of extremely large surface and high conductive pathways. A novel composite material of hierarchically structured platinum-ruthenium (PtRu) nanoparticles incorporated with 3D GF is discussed in this chapter. In this study, the preparation and characterization of 3D graphene foam incorporated with PtRu nanocatalysts are described. Th e objective of this study is to enhance the performance of PtRu nanocatalysts with carbon supporting materials as electrode materials for direct methanol fuel cells (DMFCs) and direct ethanol fuel cells (DEFCs) in anodic oxidations for energy storage and for the detection of H2O2 in biosensing.