The thermo-Raman spectra of synthesised a-gallium oxyhydroxide nanorod prove that the transition of a-gallium oxyhydroxide to b-gallium oxide nanorods occurs above 350°C but below 400°C. Scanning electron microscopy proves that the morphology of the a-gallium oxyhydroxide nanorods is retained upon calcination to b-gallium oxide. X-ray diffraction patterns show that the nanorods are a-gallium oxyhydroxide converting upon calcination to b-gallium oxide.Intense Raman bands are observed at 190, 262, 275, 430, 520, 605, and 695 cm −1 , which undergo a red shift of ∼5 cm −1 upon heating to 350°C. Upon thermal treatment above 350°C, the Raman spectrum shows a significantly different pattern. Raman bands are observed at 155, 212, 280, 430, 570, and 685 cm −1 . The thermo-Raman spectra are in harmony with the TG and DTG patterns, which show that the reaction of a-gallium oxyhydroxide to b-gallium oxide occurs at 365°C.