In this study was investigated the effect of nylon 6.6 (N6.6) nanofiber and nylon 6.6 by weight of 1%, 3% and 5% Graphene Nanoplates (GNPs) doped N6.6 nanofiber reinforced epoxy adhesives on single lap joint of AISI AA2024-T3 Aluminum Alloy (AA 2024)- Carbon Fiber Reinforced Composite (CFRC) plates. First of all, N6.6 nanofibers with/without GNPs in different proportions were produced by the electrospinning method with the help of a rotating and moving drum. Epoxy resin as the adhesive, nanofibers as the second interface to increase the strength of the epoxy and AA 2024 - CFRC were used as the bonded material and the plates cut in 101.6 × 25.4 mm according to ASTM D 1002-10 and ASTM D 5868-01, respectively. In this research was focused on the application of single lap joints by reinforcing with N6.6 nanofibres to decrease the brittleness and increase the toughness of the epoxy resin. When compared with epoxy resin, the shear strength of epoxy adhesive reinforced with N6.6 nanofibers with 3% GNPs by weight increased by 31.20%. Thermal analysis of epoxy resin and hybrid adhesives was examined by Differential Scanning Calorimeter (DSC). In addition, the physical properties of N6.6 nanofibers doped/undoped GNPs in different proportions by weight were observed with scanning electron microscopy (SEM) by damage analysis of fracture surfaces.