This study prepared the FeSe alloy using a powder metallurgy route. The Fe and Se powders were weighed at an atomic ratio of Fe:Se = 1.025:1 and milled for 5 hours. A simultaneous thermal analysis (STA) was performed to observe the behavior of the milled powder during thermal changes. After packing the milled powder in a stainless-steel tube, it was compacted. Investigation was performed to observe how the tetragonal FeSe phase forms at sintering temperatures of 718 K, 818 K, and 918 K. At a sintering temperature of 718 K, the tetragonal FeSe phase was formed, as determined by our quantitative analysis of XRD. The highest tetragonal FeSe phase fraction of 68.46 wt.% was obtained at a temperature of 918 K. The lattice constants of the tetragonal FeSe for the best sample were a = 0.3773 nm and c = 0.5520 nm. The resistivity test demonstrated that all samples have a conductor phenomenon exceeding 16 K, with a maximum Tc-onset value of 15.11 K.