Currently extensive attention on reuse and recovery of spent lithium ion batteries has been paid by researchers, especially for power applications in electric vehicles and hybrid electric vehicles, such as lithium nickel cobalt manganese oxide (NCM) batteries. In our work, a facile and green closed-cycle process with superior recovery efficiency of over 98% is proposed to recycle spent NCM materials. The metal ions are first leached out by organic acetic acid and hydrogen peroxide, and then the sphere-like NCM particles are regenerated directly from the leachate by self-made spray pyrolysis. The regenerated NCM exhibits excellent cycling retention and superior rate performance than the spent NCM and fresh NCM. The manufactured batteries display initial capacities of 157.1 and 154.3 mAh g −1 for half and full batteries, respectively, and exhibit better rate and cycling performance than those of spent NCM electrode. The investigation of spray pyrolysis will offer an innovation idea for the recycling of spent lithium ion batteries.

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Mg–Cu alloys with different phases were electrodeposited in a molten LiCl–KCl eutectic mixture containing a small amount (0.5 mol %) of MgCl2 at 673 K. The electrochemical behavior of the MgII ion and alloy formation processes were studied at inert molybdenum (Mo) and active copper (Cu) electrodes in the molten salts, respectively. Different electrochemical techniques, such as cyclic voltammetry, square‐wave voltammetry, chronoamperometry, and open‐circuit potentiometry were carried out to investigate the electrochemical formation mechanism of Mg–Cu alloys. Three signals, corresponding to the formation of metal Mg and two different Mg–Cu alloy phases, are observed when using cyclic voltammetry, square‐wave voltammetry, and open‐circuit potentiometry. Chronoamperometry studies indicate the different interfacial properties of the magnesium metal versus the Mg–Cu alloys. The results of X‐ray diffraction and scanning electron microscopy show that the MgCu2 and Mg2Cu phases could be obtained at −2.30 and −2.38 V (vs. Pt), respectively.

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