Encouragingly, a lot of research studies have demonstrated that two-dimensional (2D) nanosheets applied as an additive in oils show preferable friction-reducing and wear resistance performance. However, the current issue was that an elusive way could be adopted to probe the structure-activity relationship between the structure and tribological properties of bulk layered materials due to the structural evolution during friction testing. In this study, we studied the structure-activity relationship between the structure and tribological properties of bulk layered materials (graphite, h-BN, WS2, and MoS2) by an in situ four-ball friction tester. The morphological and structural changes of the layered materials after in situ four-ball-milling were detected by a series of characterizations. This study revealed the friction-induced nanostructural evolution behaviors of bulk layered materials by a four-ball mode.
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