In this paper, synthesis of terephthalate intercalated Zn-Al: Layered double hydroxides (LDHs) was studied. We designed freestanding Zn-Al: carbonate LDH nanosheets for a facile exchange technique. The as-prepared Zn-Al carbonate LDHs were converted to terephthalate intercalated Zn-Al:LDHs by ion exchange method. Initially, Al-doped ZnO (AZO) thin films were deposited on p-Si (001) by facing target sputtering. For synthesis of free standing carbonate Zn-Al:LDH, we dipped the AZO thin film in naturally carbonated water for 3 hours. Further, Zn-Al: carbonate LDH nanosheets were immersed in terepthalic acid (TA) solution. The ion exchange phenomena in the terephthalate assisted Zn-Al:LDH were confirmed using FTIR analysis. The crystal structure of terephthalate intercalated Zn-Al:LDH was investigated by XRD pattern analysis with different mole concentrations of TA solution and reaction times. The optimal conditions for intercalation of terephthalate from carbonated Zn-Al LDH were established using 0.3 M aqueous solution of TA for 24 hours.