Intercalated polyoxymethylene (POM)/molybdenum disulfide (MoS2) nanocomposites were prepared by in situ intercalation/polymerization. The structures of the composites were characterized by means of powder X-ray diffraction (XRD) and transmission electron microscopy. The XRD pattern showed that the polymer was inserted into the MoS2 galleries. The interlayer spacing of the intercalated phase increased from 6.15 to 11.18 angstrom. The thermal behavior of the composites was also investigated through thermogravimetric analysis. The results show that the heat resistance of the intercalated composites decreased slightly. The tribological behavior of POM/MoS2 was investigated on an MQ-800 end-face tirbometer under dry friction. The worn surfaces were observed by scanning electron microscopy. The results show that POM/MoS2 presented better friction reduction and wear resistance, especially under high load. The friction mechanism of the nanocomposites is also discussed in association with X-ray photoelectron spectroscopy. (C) 2008 Wiley Periodicals, Inc.