High-Resolution Detection of Rock-Forming Minerals by Permittivity Measurements with a Near-Field Scanning Microwave Microscope.

The identification of the minerals composing rocks and their dielectric characterization is essential for the utilization of microwave energy in the rock industry. This paper describes the use of a near-field scanning microwave microscope with enhanced sensitivity for non-invasive measurements of permittivity maps of rock specimens at the micrometer scale in non-contact mode. The microwave system comprises a near-field probe, an in-house single-port vectorial reflectometer, and all circuitry and software needed to make a stand-alone, portable instrument. The relationship between the resonance parameters of the near-field probe and the dielectric properties of materials was determined by a combination of classical cavity perturbation theory and an image charge model. The accuracy of this approach was validated by a comparison study with reference materials. The device was employed to determine the permittivity maps of a couple of igneous rock specimens with low-loss and high-loss minerals. The dielectric results were correlated with the minerals comprising the samples and compared with the dielectric results reported in the literature, with excellent agreements.

Evidence of a new phase in gypsum-anhydrite transformations under microwave heating by in situ dielectric analysis and Raman spectroscopy.

Mineral transformations of the gypsum-anhydrite system under microwave heating have been studied using in situ dielectric thermal analysis (MW-DETA) and Raman spectroscopy simultaneously. The dielectric properties of samples that were measured under microwave heating provided thorough information about the dynamics of the gypsum-anhydrite system transformations and its significance from the mineralogical point of view. In particular, the MW-DETA technique revealed a new intermediate phase with a γ-anhydrite structure. This phase corresponds to the soluble stage of γ-anhydrite, and it is characterized by a high ionic charge inside the crystal channels. The complete sequence is gypsum → 0.625-subhydrate → bassanite → hydro γ-anhydrite → anhydrous γ-anhydrite → ß-anhydrite. The transformations were also assessed using DSC, TG, DTA and dielectric measurements at room temperature, as well as other techniques including X-ray powder diffraction (XRPD) and high-temperature XRD (HT-XRD). Correlations between the dielectric properties with temperature and the rest of the techniques elucidated the heating mechanisms of this material under microwave energy during the different stages. The in situ combination of the MW-DETA and the Raman analysis appears to be a powerful technique, providing new insights about the mechanisms which govern the volumetric heating of this and other materials.