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In the present research work, the effect of varying concentration of nanoclay and un-treated/treated polyethylene terephthalate fibers (PET fibers) on tensile strength of nanocomposites was investigated. Response surface methodology (RSM) using Minitab software was used in this investigation. A total 18 experiments with 2 replications each were designed using ‘Extreme Vertices’ design model. Maximum and minimum values for tensile strength were obtained as 43.3 MPa and 26.7 MPa respectively. X-ray diffraction (XRD) analysis revealed that an intercalated structure/morphology was achieved during processing of all nanocomposites. For improvement in interfacial adhesion of PET fibers with other constituents of composite system, alkaline treatment of PET fibers was performed. For alkali treatment, different treatment times and temperatures were selected. This was followed by investigation of tensile behaviour of composites reinforced with surface-modified PET fibers treated under a given condition. SEM analysis of fractured tensile specimens was used to establish structure-property relationship. Fracture surface of tensile specimens of nanocomposites containing untreated PET fibers showed clean fiber surface and fiber pull-out locations; however, nanocomposites containing alkaline treated PET fibers exhibited fiber breakage and rough fiber surface indicating enhanced resistance to crack front growth.