Abstract
Achieving control over the phase-selective synthesis of mixed metal oxide materials remains a challenge to the synthetic chemist due to diffusion-driven growth, which necessitates the search for new compounds with pre-existent chemical bonds between the phase-forming elements. We report here a simple solvothermal process to fabricate LiCrO2 and Li2CrO4 nanoparticles from bimetallic single-source precursors, demonstrating the distinctive influence of molecular design and calcination conditions on the resulting nanomaterials. The chemical identity of [Li2Cr(OtBu)4Cl(THF)2] (1) and [LiCr(OtBu)2(PyCH=COCF3)2(THF)2] (2) was unambiguously established in the solid state by single-crystal X-ray diffraction, revealing the formation of a coordination polymeric chain in compound 1, whereas electron paramagnetic resonance spectroscopy (EPR) studies revealed a monomeric structure in solution. TEM analysis of synthesized LiCrO2 nanoparticles showed nearly uniform particles size of approximately 20 nm. The sensitivity of the LiCrO2 phase towards oxidation was investigated by X-ray diffraction, revealing the formation of the stable Li2CrO4 after calcination in air.
Highlights
The chemical synthesis of two-dimensional transition metal oxides has attracted considerable research attention due to their interesting physical, chemical, and electronic properties [1]
The growing interest in the synthesis of lower-valency chromium complexes is due to their potential applications as catalysts in ring-opening polymerization reactions and as precursors for corresponding metal oxides [10,11]
The structural features of the prepared LiCrO nanoparticles were observed by transmission The previously reported multi-source synthesis 2of LiCrO2 resulted in inhomogeneous elemental electron microscope (TEM), which showed nearly uniform grains with particles of average size 20 nm distribution and nonuniform morphologies, which could be detrimental to application of the (Figure 5)
Summary
The chemical synthesis of two-dimensional transition metal oxides has attracted considerable research attention due to their interesting physical, chemical, and electronic properties [1]. In lithium-ion batteries, the cathode materials are mostly layered compounds of lithium transition metal oxides (LiMO2 , where M = V, Cr, Mn, Fe, Co, Ni, etc.), among which Cr-based cathode materials have attracted significant attention due to possible multiple electron transfer pathways and stable cyclability, which results from the three-electron redox couple Cr3+ /Cr6+ [6,7,8,9]. LiCrO22 nanomaterials nanomaterials with with stoichiometry stoichiometry control control between between the the heterometallic heterometallic precursors precursors and and the the resulting resulting mixed mixed oxide oxide ceramics, ceramics, which which is is rather rather difficult difficult in in preparation preparation with with the the solid-state or multi-source precursor approach.
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