Two-dimensional (2D) nanomaterials, such as graphene, MoS₂, and MAX, have attracted increasing research attention in recent years due to their unique structural and performance advantages. However, their complex production processes and equipment requirements are significant issues affecting their widespread use. Here, with an exfoliation strategy using three-roll milling, we present a simple, cost-effective, and extensible method to produce multilayer graphene, BN, MoS₂, and Ti₃AlC₂ nanosheets. The roller and phenolic resin created three kinds of forces on the layered 2D materials, i.e., shear forces, compressive forces, and adhesive forces, which exfoliated layered materials from their edges and surfaces into nanosheets. Subsequently, the exfoliated materials were ultrasonically washed with alcohol, treated with ultrasonic vibration, and centrifuged to obtain 2D nanomaterials. The easy operation and high yield are attractive for research based on the construction of high-performance 2D nanosheet-based devices at low cost. Herein, the obtained multilayer graphene and MoS₂ nanosheets were used as anode materials of sodium/potassium-ion batteries, respectively, to test their electrochemical properties. Better performances are obtained compared with their primary bulk materials.

To solve the problems of low electrical conductivity and poor stability of V₂O₃ as an anode electrode of secondary batteries, sulfur (S) doped V₂O₃/C nanowires were prepared via electrostatic spinning and sulfuration treatment technology. The structure, chemical composition, and energy storage properties were characterized. The results show that the S doped V₂O₃/C nanowire as an anode electrode for lithium ion batteries has a discharge specific capacity of 538 mA·h/g at a current density of 0.1 A/g after 50 cycles, and the discharge specific capacity at 2 A/g after 600 cycles can still maintain 288 mA·h/g. The specific capacity of sodium ion batteries with S-doped V₂O₃/C nanofiber as an anode electrode is 233 mA·h/g at 0.1 A/g after 100 cycles.