The key aroma compounds in heated sheep tallow were analyzed by solvent-assisted flavor evaporation (SAFE) combined with gas chromatography-mass spectrometry (GC-MS) and gas chromatography-olfactometry (GC-O). Based on NIST2011 database search, retention index, and comparison with authentic standards, 58 volatiles were identified by GCMS, among which 2, 3-butanediol, acetic acid, acetoin, propanoic acid, hexanoic acid, and 2-hexanol were more abundant. A total of 37 odor activity regions were found by aroma extract dilution analysis (AEDA) combined with GC-O. Totally, 37 odorants were identified, among which (E,E)-2,4-heptadienal, (E)-2-nonenal, (E,E)-2,4-octadienal, (E)-2-decenal, (E,Z)-2,4-decadienal, (E,E)-2,4-decadienal, 2-heptanol, trimethylpyrazine, 4-methylthiazole, 3-(methylthio) propanal, dihydro-5-methyl-2(3H)-furanone, and 4-ethylphenol, with higher flavor dilution (FD) values (log₂FD ≥ 4), were considered to be the key aroma compounds in sheep tallow. These results can provide a basis for the utilization of sheep tallow in the food industry and the preparation of mutton flavorings.