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Energies 2022, 15, 1611 7 of 23 the cathode material is more abrasive, the 0.15 mm particle size is greatly increased, and the recovery of lithium, nickel, cobalt, and manganese is increased from 16% to 84%. Mechanochemical methods are often used in the pretreating treatment phase for the recovery of spent LIBs. Wang et al. [20] used dry ice as a co-polishing agent to destroy the crystal structure of lithium cobalt oxide (LCO) in the discharged spent LiBs cathode material under the action of mechanical force and convert it into lithium carbonate (Li2CO3) and lithium-free residue (C/Co3O4). The optimal conditions for the recovery of Li2CO3 are determined as follows: The mass ratio of dry ice to LCO is 20:1, the rotational speed is 700 rpm, and the reaction time is 1.5 h. Under these conditions, the recovery of Li2CO3 can be up to 95.04 wt%. Xie et al. [21] found that Zn powder is an effective co-grinding agent for improving the recovery of valuable metals from cathode materials. The leaching rates of Li, Ni, Co, and Mn are increased from 72.0%, 42.5%, 31.2%, and 15.2% to 99.9%, 96.2%, 94.3%, and 91%, respectively, after mechanical chemical ball milling treatment using Zn and cathode materials. The above studies show that mechanical crushing helps to leach valuable metals from spent LIBs. Most current engineering practices use mechanical crushing combined with a hydrometallurgical process to recover spent LIBs. In addition to the traditional shredding process, some researchers have proposed a more economical pretreatment process. Thompson et al. [22] suggest disassembling spent LIBs and then layering them to retain product value and simplify downstream chemicals. The shredded material can be recycled into new cathode material with cost savings of up to 20%. A similar process using disassembled batteries could save up to 80% (not considering the actual steps of disassembling the battery). As battery design progresses, separation and layering dominate because they allow for higher yields of purer products at a lower cost. It is a great method for optimizing the entire supply chain of LIBs. 3. Pyrometallurgy Treatments Pyrometallurgy is the process of separating the constituent materials of spent LIBs, which have been initially separated by physical crushing, and then subjecting them to high-temperature pyrolysis to remove the organic binder. It also allows the oxidation reduction and decomposition of the metals and their compounds in the LIBs, and then the products are recovered by different means. As shown in Figure 6, a common pyrometallurgy treatment process is summarized in this article. The valuable metals, mainly lithium, cobalt, manganese, and nickel, are extracted from the spent LIB cathode material by pyrometallurgy treatments, as concluded in Table 2. Xin et al. [23] cut the spent LIB cathode material into 2 × 2 cm pieces and roasted them in a muffle furnace at 600 ◦C to remove PVDF. The calcined cathode pieces are crushed and sieved to obtain cathode active powder. Zhang et al. [24] first used reduction roasting to directly treat the whole spent LIB and dissociate and convert the cathode material into simple substances. The hazardous electrolytes, binders, and membranes are broken down into gases and can be treated by using well-established and widely used techniques. Over 81% of the lithium can be preferentially extracted from the roasted product by aqueous carbonate leaching. Additional oxidative ammonia leaching can leach over 95% of Ni, Co, and Cu, while Mn in the ammonia leach residue can be recovered by a beneficiation process. The researchers studied the recovery characteristics of pyrolysis of used LIBs under different atmospheres. Tao et al. [25] cut the cathode material into small 5×5 cm pieces, placed the full component pieces in a tube furnace, and pyrolyzed them under a nitrogen atmosphere. The pyrolysis slag is ground and sieved to obtain a mixed powder of cathode and anode materials, which is dissolved in deionized water, and the lithium is leached using carbonic acid to obtain a lithium carbonate precipitate. The cobalt in the filtrate is leached using sulfuric acid and evaporated and crystallized to give cobalt sulfate, resulting in a final leaching filtration of 99.1% and 87.9% for cobalt and lithium, respectively. Wang et al. [26] roasted the cathode material NCM in a nitrogen (oxygen-free) atmosphere for 1.5 h at 350 ◦C and leached it with sulfuric acid, with >99% leaching of lithium, nickel, cobalt, and manganese. Yang et al. [27] roasted the cathode powder under a methanePDF Image | Recycling of Lithium Batteries
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