Transmission Electron Microscopy Analysis of Mo–W–S–Se Film Sliding Contact Obtained by Using Focused Ion Beam Microscope and In Situ Microtribometer

To better understand the fundamentals of solid lubrication, microstructural analyses on the wear scar surface and contact interface of Mo–W–S–Se composite films produced by pulsed laser deposition were completed. Focused ion beam (FIB), transmission electron microscopy (TEM), and X-ray energy dispersive spectroscopy were employed to study the cross-sectional microstructure and chemistry of wear scars. In particular, a novel microtribometer was built for in situ tribological measurements within a FIB microscope. The sliding tip was welded in contact to the wear scar surface on the film under load by re-deposition of sputtering materials from the FIB cut of the tip. Using this technique, cross-sectional TEM specimens were prepared precisely at the contact point without tip/film separation. Here, the in situ FIB microtribometer is critically important for retaining the microstructure of lubricant films as formed at the sliding contact interface between the tip and film without separation. It provides the unique ability to stop sliding, section the contact, and reveal microstructural changes to that contact without disrupting the sliding interface. The cross-sectional TEM measurements were performed on the sliding contact interface for both the regions in contact and just past contact, and both the reorientation and recrystallization of lubricant films were revealed.