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In this scientific research, thermally stable nickel nanoparticles were synthesized and characterized. Nickel nanoparticles were synthesized using phenol –formaldehyde by chemical method followed by calcination. The polymer metal complex was confirmed by FTIR and NMR. The spherical morphology of nickel nanoparticles confirmed by SEM. The crystallographic structure is confirmed by XRD and size of cobalt nanoparticles is 24.0 nm. The TGA analysis was performed over a range of 29-600OC. Thedoi:10.20944/preprints202007.0391.v1 fatcat:xgfgrfy4tbdbnimwsuuhyhnkkm