The inorganic and organic nanocomposites have enticed wide interest in the field of polymer-based composite systems to augment their physiochemical properties like mechanical strength and electrical conductivity. Achieving interfacial interaction between inorganic filler and polymer matrix is a recurring challenge, which has significant implications for mechanical properties of nanocomposites. In this context, the effect of "interfacial zone" on structural and thermal attributes of the melt blended pristine polycarbonate and polycarbonate (PC) decorated fumed silica nanocomposite have been examined from ambient temperature to the glass transition temperature. Thermomechanical characterization and in-situ temperature assisted small angle X-ray scattering technique (SAXS) were used for contemplating quantitative and qualitative molecular dynamics of developed nanocomposites. Though, the FT-IR spectra have demonstrated some extent of interaction between inorganic and organic groups of composite, the reduced glass transition temperature and storage modulus was ascertained in DMA as well as in DSC, which has been further confirmed by in-situ temperature assisted SAXS. It is envisioned that the utilization of in-situ SAXS in addition to the thermomechanical analysis will render the qualitative and quantitative details about the interfacial zone and its effect on thermal and mechanical properties of nanocomposite at varying temperature conditions.