Characterization of the Powders Reported to Contain Polycrystalline Glitter and Silicon Dicarbide

Bucknum and Stamatin reported the synthesis of powdered, polycrystalline glitter and silicon dicarbide, heretofore hypothetical phases, in June, 2003. The synthesis was accomplished with the use of high temperature (>1400 K) using starting materials consisting of Novolac resin, a phenol-formaldehyde condensation resin similar to Bakelite, and a crosslinking agent called hexamethylenetetramine (HMTA) that is a rich source of reactive methylenes. Silicon powder was added to some of the reaction mixtures to promote the synthesis of silicon dicarbide, isostructural to the carbon allotrope glitter. The authors used x-ray diffraction (XRD) and transmission electron microscopy (TEM) to characterize their synthesis products of the thermal treatment, and provided evidence for their synthesis. The present report describes an independent analysis of the reaction products of Stamatin et al. as they occurred in polycrystalline, powdered samples. This independent analysis was carried out at the A.J. Drexel Nanotechnology Institute under the direction of Gogotsi. It utilized XRD, Raman spectroscopy, scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDS) to characterize the samples and show that an alternative explanation of the XRD data is possible.