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ll iScience OPEN ACCESS Figure 1. Morphology of LMO Nanotubes (A–C) (A) SEM image and (B and C) TEM images of LMO nanotubes at different magnifications. et al., 2016). The collapse of the spinal structure, triggered by the MnII/MnIV dissolution, degrades the per- formance and reusability of the sorbent. Therefore, the acidic treatment poses a persistent challenge for LMO implementations of lithium exploitations. The interest in applications of nanostructured sorbents for lithium extraction is attributed to its high surface area and high adsorption capacity (Du et al., 2016; Kamran et al., 2019; Luo et al., 2016). However, relatively poor stability has been achieved. The adsorption performance strongly depends on the morphology, porosity, and crystalline structure of the material (Xu et al., 2016). One-dimensional nanomaterial with enlarged surface area and accessible extraction-desorption sites is promising for lithium recovery (Moazeni et al., 2015). The nanostructured network facilitates favorable ion transportation, thus allowing high Li+ up- date capacity and fast recovery kinetics (Tang et al., 2013; Wu and Zhao, 2011). It has been demonstrated that single-crystalline material boosts efficient and reversible lithiation/delithiation processes due to its well-defined geometry, short Li+ ions diffusion length, and perfect crystallization (Ding et al., 2011). In this study, we synthesized a single-crystalline LMO nanotube, with a composition of Li1.1Mn1.9O4, for the selective recovery of Li+ from LiCl solutions and simulated brines. The reusability and adsorption perfor- mance of LMO nanotubes was ensured using ammonium persulfate ((NH4)2S2O8) as the eluent. RESULTS Figure 1A shows a typical Scanning Electron Microscope (SEM) image of LMO nanotubes prepared by a template-engaged synthesis using b-MnO2 nanotubes as the precursor. The LMO nanotubes exhibited a length and a width in a range of 0.5–2 mm and 70–200 nm, respectively. The interior hollow structure of LMO nanotubes was observed by Transmission electron microscope (TEM) (Figures 1B and 1C). The forma- tion of b-MnO2 templates (Figures S1A and S1B, Supplemental Information), based on the hydrothermal process, encompasses through a nucleation-dissolution-anisotropic growth-recrystallization mechanism. The growth of b-MnO2 tubular structures involves the dissolution and recrystallization of g-MnOOH as in- termediates. The tips of b-MnO2 templates exhibit a sharp boundary as the material undergoes a phase transition from the intermediates to b-MnO2, leading to a tubular nanostructure (Figures S1C and S1D, Supplemental Information). This morphology is effectively maintained during the subsequent solid-state reaction (Figure 1B). The aspect ratio of nanotubes is increased, indicated that the tubes slightly swell in the direction perpendicular to the tube axis through the template-engaged transformation process. High-resolution TEM results reveal a single-crystalline structure of LMO nanotube, with an inner and outer diameter of 48 and 70 nm, respectively (Figure 1C). The composition and crystal structure of obtained LMO nanotubes were analyzed by Inductively Coupled Plasma-Optical Emission Spectroscopy (ICP-OES) and X- ray Diffraction(XRD) characterizations. The nanotubes demonstrated a well-crystallized cubic spinel struc- ture with the Fd3m symmetry (Figure S2, Supplemental Information). The lattice constant is calculated to be 8.239 A ̊ , which is slightly smaller than that of the literature value (8.248 A ̊ , JCPDS No. 35–0782), implying that partial manganese sites might be occupied by lithium in the spinel lattice. The assumption is supported by ICP-OES measurements. The results showed that the atomic ratio of Li:Mn is 0.578, indicating that a lithium- rich phase of Li1.1Mn1.9O4 is obtained by the reaction between nanotube templates and LiOH at the high temperature. The extra Li+ in interstitial sites of the lithium-rich manganese oxide improves the structural stability and allows higher Li+ uptake capacity (Bajestani et al., 2019; Chitrakar et al., 2001; Xiao et al., 2013). It is found that the Brunauer-Emmett-Teller(BET) surface area of LMO nanotubes is 121.3 m2 g1 (Figure 2), with an average pore size around 50 nm determined by the Barrett-Joyner-Halenda method, which is in good agreement with TEM analysis. Article 2 iScience 23, 101768, November 20, 2020PDF Image | Extraction of Lithium from Single-Crystalline Lithium
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