Structural and spectroscopic characterization of keatite (SiO₂)

Abstract

Keatite, a polymorph of silica rare in nature, was synthesized by hydrothermal treatment of silicon and water at 100 MPa and 600 °C. The crystal structure of keatite at 24 °C was refined by the Rietveld method using synchrotron X-ray diffraction data. The obtained structure is consistent with the results of previous studies in which some constraints were imposed during refinements. The ²⁹Si MAS NMR spectrum of keatite shows two peaks at −113.9 and −114.3 ppm, which can be assigned to Si at the Si1 and Si2 sites, respectively. The Raman spectrum of keatite shows a prominent peak at 473 cm⁻¹, which is attributable to the Si–O–Si bending mode of the 5-membered ring. These spectra, reported for the first time, are expected to be valuable for the identification of keatite in synthetic and natural samples.