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iScience ll Article Figure 2. A Nitrogen Adsorption-Desorption Isotherm of Single-Crystalline LMO Nanotubes The inset shows the corresponding pore size distributions obtained using the Barrett-Joyner-Halenda (BJH) method. To understand solid-state reactions, we investigated the XRD patterns for the b-MnO2 nanotube and the calcined products, obtained at 500, 600, and 700C respectively (Figure 3). The diffraction peaks of nano- tube templates are indexed for the tetragonal structure of b-MnO2 (JCPDS 24–0735, space group P42/ mnm) without any impurity peaks. Lithium ions enter the square channels of tetragonal b-MnO2 via solid-state reactions. The reduction of MnIV to MnIII leads to the lattice expansion owing to the larger radius of MnIII than MnIV phase, accompanied by the formation of LiO4 tetrahedra and new MnO6 octahedra. As XRD results showed, the calcination triggers the reorganization of structure owing to the strongest diffract peak corresponding to (110) reflections of b-MnO2 disappeared. The transformation is facilitated by the high mobility of Li+ ions at elevated temperatures (Lu et al., 2019). While LMO500 and LMO600 show the presence of a-Mn2O3 phase, an undistorted cubic bixbyite with Ia3 symmetry (Figure S3, Supplemental Information); the reaction at 700C complete phase transformation from tetragonal b-MnO2 to spinel Li- rich structure. The SEM images of the products prepared at different temperatures showed the nanotube morphology is preserved (Figure S4, Supplemental Information). Despite the impurities were identified at the surface of LMO nanotubes calcined at 500C (Figures S4A and S4D), the materials show a uniform tubular morphology upon increasing the temperature. The dimension of LMO nanotubes does not change evidently over the solid-state reaction (Figures S4A–S4C). It has been suggested that the tetragonal-to-cu- bic transformation requires a cooperation jump to a nearest-neighbor site of half the cation array, followed by an adjustment of the Mn-O distances to convert the tetragonal anion packing of rutile to the cubic close packing of anions in the spinel structure (David et al., 1984). The adjustment sustained a minimal reorga- nization of structure in the tetragonal precursor, generated a more stable spinel LMO framework with a higher symmetry than that of the nanotube templates. Therefore, the tubular nanostructure and high crys- tallinity of the precursor were preserved through solid-state reactions. Spinel LMO nanotubes, prepared by b-MnO2 nanotube and LiOH at 700C, were selected for Li+ adsorp- tion/desorption tests followed by the experimental procedure shown in Figure S5 (Supplemental Informa- tion). Figure 4A presents the elution curves, accompanied by manganese dissolution, for LMO nanotubes delithiated by 0.5 M H2SO4 and (NH4)2S2O8. The results showed that the (NH4)2S2O8-eluted LMO nano- tubes exhibited significantly low manganese dissolution and slightly decreased Li+ recovery kinetics, as compared to H2SO4-eluted LMO. To elucidate the advantages of single-crystalline nano-tubular structure, we tested the extraction performance of commercial LiMn2O4 materials purchased from Aldrich (Figures S6A and S6B, Supplemental Information). The commercial LMO particles exhibit moderate kinetics and low Li+ uptake capacity (Figure S6C, Supplemental Information), whereas Li+ uptake capacity of LMO nano- tubes was initially high and then steadily reached for an equilibrium. The (NH4)2S2O8-eluted LMO nano- tubes showed low manganese dissolution due to the hydrolysis of S2O82, where the peroxy bond breaks into SO, free radicals (Equation 1) (Marthi and Smith, 2019). The SO,=SO2 transformation (Equation 2) 444 OPEN ACCESS iScience 23, 101768, November 20, 2020 3PDF Image | Extraction of Lithium from Single-Crystalline Lithium
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