Abstract Imogolite (Imo) was prepared via a sol-gel method. The time-dependent changes in its morphology, structure and texture during the whole synthesis process (from amorphous precursors to the final products… Click to show full abstract
Abstract Imogolite (Imo) was prepared via a sol-gel method. The time-dependent changes in its morphology, structure and texture during the whole synthesis process (from amorphous precursors to the final products through nanoscale intermediates) were monitored by atomic force microscopy (AFM), X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, nuclear magnetic resonance (NMR) and N2 physisorption. The results showed that a shape transition from a spherical open imogolite local structure (ImoLS) to a tubular open ImoLS occurred in the process of proto-imogolite (proto-Imo) formation. Based on the overall structure of the obtained solid products and the occurring main reactions, Imo synthesis process was described in five steps: i) formation of amorphous precursors by hydrolysis and condensation of Al and Si; ii) formation of proto-Imo with an open ImoLS at the expense of the amorphous precursors; iii) open ImoLS dominates; it grows and assembles into the first closed ImoLS (tubes and spheres); iv) closed ImoLS dominates and continues to form (mainly tubes) at the expense of open ImoLS; and v) no more open ImoLS; further growth of already-formed Imo via oriented aggregation. These findings provide new insights into the formation mechanism and structure of proto-Imo and Imo, which helps to clarify the Imo synthesis procedure.
               
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