The electrode materials from spent lithium-ion batteries consist of graphite and lithium cobalt oxides (LCO), which cannot be efficiently separated by the conventional flotation technique due to the fine size distributions of graphite and LCO. In this work, nanobubbles were introduced to the flotation system of electrode materials. Nanobubbles were produced with the method of temperature difference. Different degrees of gas oversaturation in the water/slurry were achieved by raising the temperature of cold water (stored at 4 °C for at least 72 h) to target values of 20 °C, 25 °C, and 30 °C. It was found that the height and lateral distance of nanobubbles increased with the degree of gas oversaturation of water. In addition, the larger graphite agglomerations were observed to form in the presence of nanobubbles. The D₅₀ (chord length) of graphite agglomerations increased by 8 μm, 11 μm, and 21 μm, respectively, compared with the D₅₀ of graphite in natural water. More graphite agglomerations adhered to a captive bubble with the aid of nanobubbles than in the case of no nanobubbles, which was indicated by increased wrapping angles of graphite (agglomerations) adhering to a captive bubble. Furthermore, the maximum adhesion force between a captive bubble and substrate increases to 220, 270, and 300 μN as cold water temperature increases to 20, 25, and 30 °C, respectively. The frost of nanobubbles on a graphite surface and the resulting graphite agglomerations through the bridging effect of nanobubbles are thought to be responsible for the improved flotation performance of electrode materials. The present results indicate that the flotation performance of fine minerals can be regulated by regulating the gas oversaturation degree of the slurry.

Regulating the dissolution and interfacial behavior of minerals via external force fields is considered a promising strategy for enhancing the flotation of soluble minerals. This study explored the potential of ultrasound-assisted pulp conditioning in improving ultrafine smithsonite flotation. Specifically, we systematically evaluated the effects of ultrasonic pretreatment (UP) on the physicochemical properties of smithsonite suspensions (focusing on surface erosion behavior) and assessed subsequent flotation performance using flotation tests and modern analytical techniques. It has been found that UP can significantly modify smithsonite suspension characteristics, including particle morphology, ionic composition, electrokinetic properties, and pulp pH. Flotation results demonstrate that UP yields higher recovery compared to traditional stirring (TS) conditioning, especially at medium-to-high sodium oleate (NaOL) concentrations. Comparative analysis reveals that ultrasonic-assisted dissolution and ion-selective migration are the main factors driving improved flotation performance. Unlike TS, UP promotes greater zinc ion release, facilitates the dissolution–hydrolysis–precipitation equilibrium, generates more and finer nanoparticles in the bulk phase, and induces the deposition of hydrozincite on smithsonite surfaces. These changes increase active zinc sites for more stable NaOL adsorption, thereby enhancing the flotation of ultrafine smithsonite particles.