The present studies were focused on the analysis of thermal and biological properties of various metal composites of [4-N-Phenylethanamide azo-3-N-(4-chlorophenyl) maleimide-co-Acrylic acid] [CPAChMI-AA], [4-N-Phenylethanamide azo-3-N-(4-Bromophenyl) maleimide-co-Acrylic acid] [CPABMI-AA].The monomers [4-N-Phenylethan amide azo-3-N-(4chlorophenyl)Maleimide] [PAChMI], [4-N-Phenylethanamide azo-3-N-(4-bromophenyl)Maleimide] [PABMI] and copolymers [CPAChMI-AA] and [CPABMI-AA] were synthesized. The monomers were made by reaction with maleic anhydride and substituted amino-derivative as 4-N-Phenyl ethanamide via dehydration-cum-cycloaddition reaction process and copolymerized with acrylic acid at 60-70 o Cin tetrahydrofuran (THF) solution using initiator as azoisobutyronitrile (AIBN). Metal composites of synthesized copolymers were prepared with some metals such as Co 2+ , Ni 2+ , Cu 2+ , Fe 2+ . All compounds were characterized by means of FT-IR, 1H-NMR, elemental analysis and DSC and TGA evaluated thermal properties of polymers and their metal composites. Molecular weight and polydispersity were determined by gel permeation chromatography (GPC). Biological performances were examined in the form of microbial activities of the polymers and composites with various bacteria / fungi.