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This study examined the tribological performance of three gear oils (Oils A, B and C), in relation to surface and microstructural changes. Oil A contains molybdenum dithiophosphate friction modifier, Oil B contains amine molybdate combined with zinc dialkyl dithiophosphate antiwear additive, while Oil C contains phosphonate and a commercial gear oil package. Following sliding tests of a hardened AISI 52100 steel ball on a spheroidized AISI 52100 steel disc, the worn surfaces were chemically studied using Raman and energy-dispersive X-ray spectroscopy. The tribological performance for each oil was different, likewise the nature of the tribofilm formed. After a 5 min sliding test, the hardness-depth profile of the worn surfaces was measured; also the cross-sectional microstructure was examined using scanning electron microscopy combined with focused ion beam preparation and transmission electron backscattered diffraction (t-EBSD) techniques. With Oil A, there was a relatively small increase in surface hardness (33% greater than that of the unworn surface), whereas with Oils B and C, the average hardness near the surface was 100% greater than that of the unworn surface. The cross-sectional microstructure using Oil A also differed from Oils B and C, which were quite similar. The result shows that with Oil A refinement of the ferrite grains spreads deeper into the material (> 10 µm), whilst with Oils B and C it was largely limited to 2–3 µm below the surface. It is concluded that the lubricant formulations and their associated tribofilms influenced the extent of deformation in the subsurface layers and consequently influenced the wear performance.