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iScience ll Article OPEN ACCESS Figure 4. Extraction and Recovery Performance of LMO Nanotubes (A and B) (A) Elution tests and (B) regeneration tests of Li extraction, along with Mn dissolution, for LMO nanotubes eluted by 0.5 M H2SO4 and (NH4)2S2O8. (C–E) (C) XRD results of pristine LMO, H2SO4-eluted, and (NH4)2S2O8-eluted LMO nanotubes, respectively. Rietveld refinement of (D) H2SO4-eluted and (E) (NH4)2S2O8-eluted LMO nanotubes after eight adsorption/desorption cycles. (F) Schematic illustration of the lithium uptake for adsorption/desorption processes. topotactically. Rietveld refinements were used to analyze the XRD results of H2SO4-eluted and (NH4)2S2O8- eluted LMO nanotubes (Figures 4D and 4E). LMO nanotubes, eluted by 0.5 M H2SO4 and (NH4)2S2O8, exhibit a lattice parameter of 8.032 and 8.054 A ̊ , respectively, indicating a larger volume change for H2SO4-eluted LMO nanotubes (Table 1). While the pristine LMO showed a Li-rich spinel structure after solid-state reactions, the ratio of Li/Mn is reduced due to Mn dissolution after eight adsorption/desorption cycles (Table 1). It has been known that adequate MnIII/MnIV ions in the spinel structure are necessary to maintain the ideal cubic dense packing state of O atoms in each layer, forming a Mn2O4 skeleton which is favorable for Li+ diffusion (Figure 4F) (Ben et al., 2017). The Li+ extraction at the 8a position of the LMO through the path of 8a16c8a. The Jahn-Teller effect may occur during the adsorption/desorption process that the repeated insertion/extraction of Li+ causes the deformation and even collapse of the spinel structure (Ragavendran et al., 2017). Figure 5A showed that X-Ray Photoelectron Spectroscopy(XPS) spectra of Mn 2p1/2 and Mn 2p3/2 for pris- tine LMO and LMO nanotubes, eluted by H2SO4 and (NH4)2S2O8. The shift of binding energy is attributed to the lattice distortion of manganese-oxygen bonds (Qian et al., 2020). The valence analysis was per- formed by deconvolutions of Mn 2p3/2 spectra (Figure 5B). The results indicated that the ratios of Mn4+:Mn3+ on the surface are 51.0%:49.0%, 44.9%:55.1%, and 46.8%:53.2% for pristine LMO, H2SO4-eluted, and (NH4)2S2O8-eluted LMO nanotubes, respectively (Table 1). While eluted LMO nanotubes exhibit an in- crease of Mn3+, (NH4)2S2O8-eluted LMO nanotubes showed higher valence state of Mn compared to H2SO4-eluted LMO nanotubes. The reduction of Mn triggered dissolutions of Mn2+ in acid solutions during the extraction process (Gao et al., 2018). It is suggested that as the average valence state of Mn decreased lower than +3.5, the cubic crystal changes to tetragonal, while the tetragonal phase showed irreversible transformations of Li+ adsorption/desorption (Abuzeid et al., 2018). The improved recovery performance of LMO nanotubes is attributed to higher chemical stability and less volume changes for the acid-free processing. The acid-free method was employed for Li+ recovery from simulated brines. (NH4)2S2O8-eluted LMO nano- tubes exhibited a high selectivity of Li+ from the brine, containing Li+, Na+, K+, and Mg2+ ions under the iScience 23, 101768, November 20, 2020 5PDF Image | Extraction of Lithium from Single-Crystalline Lithium
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Product and Development Focus for Infinity Turbine
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