Abstract
Porous Ge@C materials as anode materials for Li-ion batteries were synthesized by the novel concept of twin polymerization starting from germylenes based on salicyl alcoholates.
Highlights
The as-obtained germanium-containing phenolic resin hybrid materials (HM-1– HM-3) and the consecutively synthesized GeO2 and germanium incorporated in a carbon matrix (Ge@C) materials were characterized by analytical techniques such as solid state NMR spectroscopy (HM-1–HM-3), X-ray photoelectron spectroscopy (XPS), infrared (IR), Raman and energy-dispersive Xray (EDX) spectroscopy, powder X-ray diffraction (PXRD), nitrogen-sorption, measurements transmission electron microscopy (TEM) and CHN analysis
The germylenes 1–3 were prepared according to the synthesis protocol of 4 starting from Ge[N(SiMe3)2]2 and the respective salicyl alcohol with yields in the range from 64% to 73%
Poor solubility in non-polar solvents was observed for germylene 3, whereas the compounds 1 and 2 are soluble in all common organic solvents. 1H NMR and 1H13C{1H} HSQC NMR spectroscopic analysis of freshly prepared solutions of the germylenes 1–3 in d8-THF at ambient temperature gave broad resonance signals indicating a dynamic coordination behavior including oligomeric species, presumably dominated by their monomers
Summary
Scheme 1 Illustration of the basic structural motif of the germylenes 1–4 (n 1⁄4 2–4) and the concept for the synthesis of e.g. a porous Ge@C material for rechargeable Li-ion batteries starting from 1–3 according to the concept of twin polymerization followed by reduction of the hybrid material. The substituent in the para positions of their phenolate moieties possess distinguishable steric and electronic features, which is expected to in uence their reactivity towards TP as reported for spirocyclic salicyl alcoholates recently.[65] Characterization including single crystal X-ray diffraction analysis and DFT-D calculations, and studies on their reactivity in TP using differential scanning calorimetry (DSC) are presented. Ge@C materials as obtained starting from germylene 1 were tested as anode materials for rechargeable Li-ion batteries and their performance is discussed
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