Mono-dispersed molybdenum disulfide micro-spheres with the diameter of 1–3 μm have been successfully synthesized via extraction–solvothermal method at 150 °C. The extractant Cyanex 301 (di-(2,4,4-trimethylpentyl) dithiophosphinic acid) acted as phase transferring agent, reductant, sulfur source and morphology-controlling agent in the whole procedure. The obtained MoS 2 micro-spheres were characterized by XRD, EDS, SEM, TEM, HRTEM, IR, UV-Vis and TG, respectively. The influences of reaction conditions were discussed while a mechanism was proposed to explain the formation of the micro-spheres. Moreover, the tribological properties of liquid paraffin (LP) containing Cyanex 301-modified MoS 2 micro-spheres were also evaluated on a four-ball machine, showing that the obtained MoS 2 product was an excellent oil additive in LP and such lubricant had good anti-wear and friction-reducing properties.
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