Observation of the transformation of silica phytoliths into SiC and SiO2 particles in biomass-derived carbons by using SEM/EDS, Raman spectroscopy, and XRD
2019
Yapuchura, Enrique R. | Tartaglia, Rodolfo S. | Cunha, Alfredo G. | Freitas, Jair C. C. | Emmerich, Francisco G.
Scanning electron microscopy coupled to energy-dispersive X-ray spectroscopy, Raman spectroscopy, and X-ray diffraction were successfully used to observe the location and morphology of the silica phytoliths in biomass-derived carbons and their transformation into SiC and SiO₂ particles at high heat treatment temperatures (HTT). The analyses were conducted in chars derived from the endocarp of babassu coconut (EBC), which naturally contains 1.6 wt% of silica in its mineral matter. It was observed that EBC chars with 500–1200 °C HTT present globular echinate SiO₂ phytoliths with sizes of 12–16 μm; these phytoliths are mostly concentrated around the surface of the submillimeter char fibers and also in the carbonaceous char matrix. No phytoliths are found in the interior of the char fibers. At 1200 °C HTT, the phytoliths begin to be rounded, and above 1300 °C HTT, most phytoliths decompose and silicon reacts with carbon-forming nanocrystalline β-SiC particles (~ 35 nm crystallite size). Numerous (tens to hundreds) micro- and sub-micro-amorphous or nanostructured SiO₂ particles (with sizes predominantly below 2 µm) are then observed at the sites previously occupied by the phytoliths. Few rounded phytoliths survive at 1400 °C HTT, but disappear at higher HTTs (1600–2000 °C). It is likely that the ensembles of micro- and sub-micro-SiO₂ particles observed in many sites correspond to the inner remaining part of the original phytoliths, whose most external SiO₂ structures (at and near the surface) decompose and take part in the carbothermal reaction for the formation of SiC.
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