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Primary intent of the present paper is to correlate the effectiveness of surface preparation type (pre-bonding), such as solvent cleaning, sanding (mechanical abrade), chemical etching (alkaline and acid), and peeling of sacrificial surface layer (peel ply) of carbon fiber reinforced composite (CFRC) test specimens, with the corresponding effect to the final strength of adhesive bonding. The analysis was performed by means of several spectroscopic and microscopic techniques, such as XPS, SEM, AFM, and a contact angle measurement technique which provides a direct, fast and easy measurement of the surface energy of the fiber composites. The adhesively bonded carbon fiber composites based on the different surface treatments were mechanically tested by employing the ASTM D 5528-0 (reapproved 2007) standard. The double cantilever beam (DCB) specimen geometry was used to evaluate the value known as opening Mode I inter-laminar fracture toughness (GIC) in adhesive bonds of carbon fiber composite materials. The results were varying between 1 and 1.8 kJ/m2 for GIC analysis and around 50 mm for delamination lengths. The mechanics of the linear elastic fracture is considered a tool for the failure of the laminate in composite materials with cracks or cuts in the plane, due to the presence of damaged zones in the tip of the crack; which is therefore applied to the study of delamination or fracture toughness.