Phase transitions of ferruginous minerals in the course of thermal processing of feldspar-quartz raw materials from the Sobótka region (Lower Silesia)

This paper presents the results of analyses of feldspar-quartz raw materials from deposits of leucogranites located in the Sobótka region. This is a successive stage of research carried out by the author on reasons for colour variation of ceramic materials obtained from them. This step encompassed the firing of sample pairs of analogous chemical composition in different conditions: in a standard cycle lasting more than 2 hours (at a maximum temperature of 1200°C), and a fast one - lasting around 50 minutes (at a max. temperature of 1260°C). The obtained ceramic bodies were analysed using the XRD method, scanning microscopy SEM-EDS and 57Fe Mössbauer spectroscopy at room temperature. The XRD investigations revealed the presence of quartz in both samples, while remnants of sodium feldspar were observed in the one fired in the fast cycle. The scanning microscopy confirmed that the principal component of the examined bodies is the aluminosilicate melt, resulting from the thermal decomposition of mainly feldspars and quartz. Single quartz grains and other minerals of high melting temperatures, i.e. zirconium, were also observed in the course of microscopic examinations. Products of other mineral phases’ transformations at high temperature, such as: titanomagnetite (spinel Fe-Ti), magnetite, biotite, xenotime, sphalerite as well as probably chlorites and garnets, were also relatively frequent. Mössbauer studies demonstrated the presence of three basic components constituting 30% (each) of the spectra, i.e. Fe2O3 (presumably hematite), Fe3+ ions (dispersed in aluminosilicate glassy phase), and nanocrystalline or amorphous oxide phase of iron (Fe-O). Some relatively small amounts (5 and 10%) of mixed valence iron cations (Fe2+/3+) that are not expected to influence the colour difference between samples after firing were also found. A paramagnetic doublet referring to them can be attributed to a titanomagnetite spinel or products of its thermal decomposition. The above-mentioned observations and examinations lead to the finding that the main reason for colour variation in the examined bodies as well as their different microstructure and advancement of phase transitions in the course of firing are different conditions of thermal treatment. These probably also influenced the forms in which iron and other colouring elements occur in the samples studied.