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• W2971986343 abstract "Gibbsite (α-Al(OH)3) transformation into layered double hydroxides, such as lithium aluminum hydroxide dihydrate (LiAl-LDH), is generally thought to occur by solid-state intercalation of Li+, in part because of the intrinsic structural similarities in the quasi-2D octahedral Al3+ frameworks of these two materials. However, in caustic environments where gibbsite solubility is high relative to LiAl-LDH, a dissolution-reprecipitation pathway is conceptually enabled, proceeding via precipitation of tetrahedral (Td) aluminate anions (Al(OH)4-) at concentrations held below 150 mM by rapid LiAl-LDH nucleation and growth. In this case, the relative importance of solid-state versus solution pathways is unknown because it requires in situ techniques that can distinguish Al3+ in solution and in the solid phase (gibbsite and LiAl-LDH), simultaneously. Here, we examine this transformation in partially deuterated LiOH solutions, using multinuclear, magic angle spinning, and high field nuclear magnetic resonance spectroscopy (27Al and 6Li MAS NMR), with supporting X-ray diffraction and scanning electron microscopy. In situ27Al MAS NMR captured the emergence and decline of metastable aluminate ions, consistent with dissolution of gibbsite and formation of LiAl-LDH by precipitation. High field, ex situ6Li NMR of the the progressively reacted solids resolved an Oh Li+ resonance that narrowed during the transformation. This is likely due to increasing local order in LiAl-LDH, correlating well with observations in high field, ex situ27Al MAS NMR spectra, where a comparatively narrow LiAl-LDH Oh27Al resonance emerges upfield of gibbsite resonances. No intermediate pentahedral Al3+ is resolvable. Quantification of aluminate ion concentrations suggests a prominent role for the solution pathway in this system, a finding that could help improve strategies for manipulating Al3+ concentrations in complex caustic waste streams, such as those being proposed to treat the high-level nuclear waste stored at the U.S. Department of Energy's Hanford Nuclear Reservation in Washington State, USA." @default.
• W2971986343 created "2019-09-12" @default.
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• W2971986343 date "2019-09-05" @default.
• W2971986343 modified "2023-09-27" @default.
• W2971986343 title "Unraveling Gibbsite Transformation Pathways into LiAl-LDH in Concentrated Lithium Hydroxide" @default.
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• W2971986343 doi "https://doi.org/10.1021/acs.inorgchem.9b02000" @default.
• W2971986343 hasPubMedId "https://pubmed.ncbi.nlm.nih.gov/31486636" @default.
• W2971986343 hasPublicationYear "2019" @default.
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