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We report on the preparation of two‐dimensional (2D) Ti3C2 and its friction and wear properties. Laminated Ti3AlC2 was synthesized by pressureless sintering using Ti, Al, and graphite, followed by HF exfoliation and sonication treatment to form 2D‐layered Ti3C2, which exhibited individual layer or stack of several layers. Analysis of microstructure and composition was used to confirm the successful exfoliation of laminated Ti3AlC2. The tribological behaviors of the as‐prepared 2D Ti3C2 as a lubrication additive in base oil were investigated. Results indicate that 2D‐layered Ti3C2 can greatly enhance the friction‐reducing and anti‐friction properties of base oil, especially with 1.0 wt% Ti3C2. This novel 2D‐layered Ti3C2 would be a good candidate for lubricating materials to meet emerging needs in practical applications.

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TiO2/Ti3C2Tx hybrid nanocomposites were successfully prepared by a liquid phase synthesis technology. The hybrid nanocomposites improve the tribological properties of base oil by mending the surface and formation a uniform tribofilm on the surface.