A hybrid protein fiber from different protein sources such as casein and soybean using wet-spinning technique was prepared. The casein/soybean hybrid fibers were synthesized at different weight ratios such as 100/0 (casein), 75/25, 50/50, 25/75, and 0/100 (soy) and characterized. Electron microscopic analysis confirmed the growth of pure and hybrid fibers and shows an increased surface roughness as the soy concentration increases in the hybrid fibers. Infrared spectra did not exhibit any significant changes in the functional groups between pure and hybrid fibers. X-ray diffraction pattern indicates slight increase in the diffraction peak values of hybrid fibers compared with the neat fibers. Thermal analyses show a moderate increase in the thermal stability of hybrid fibers when compared with the pure fibers. These results implicitly indicate that the casein and soy proteins are homogeneous in the hybrid fiber form. It has been demonstrated that the hybrid fiber with ≥50 wt.% casein content exhibits better morphology and increased thermal stability, which has scope for application in technical and medical industries.