Boron nitride nanosheets (BNNSs) possess many unmatched properties, including satisfactory thermal conductivity and stability, excellent mechanical performance, and wide band gap. Nevertheless, the highly efficient exfoliation and functionalization of BNNSs still remain an enormous challenge. In our work, we presented a facile synergistical exfoliation and functionalization method to acquire OH-functionalized BNNSs (BNNS-OH) via calcination, plasma treatment, and ultrasonic exfoliation with a high yield and a large concentration. Under the optimized conditions, the yield and dispersion concentration of BNNS-OH can reach 80.1% and 5 mg/mL, respectively. In addition, the as-prepared BNNS-OH could be used as a green water-based lubricant nanoadditive and corrosion inhibitor on metals, which decreased the friction coefficient from 0.350 to 0.335 and corrosion current density from 3.54 × 10 −4 A/cm 2 to 1.38 × 10 −4 A/cm 2 . More importantly, this proposed synergistical exfoliation and functionalization method proved to be a universal method for the exfoliation and functionalization of other two-dimensional materials such as graphite and boron.
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