The aim of this study has been to analyse the mineralogical and textural transformations of a set of aluminiumrich shales of interest for refractory and ceramic uses, fired from 800°C to 1300°C. To that end, raw and fired samples were analysed by X-ray diffraction, transmitted light microscopy, field emission scanning electron microscopy, and transmission electron microscopy. Raw samples comprise variable proportions of illite, pyrophyllite, orthoclase, quartz, kaolinite, mixed-layer I-Sm, and organic matter. At temperatures below 800°C, kaolinite, mixed-layer I-Sm, and organic matter are destabilized, indicating that they are the least stable phases in the firing process. Illite, pyrophyllite, and orthoclase remain until 1000°C and show a broader stability field during firing than in natural environments. Quartz persists throughout the entire firing process, although it is partly replaced by vitreous phase. Hematite crystallizes at 900°C. Vitrification begins at 1000°C, marking the first significant textural change. From 1000°C mullite starts to crystallize from the Si-and Al-rich vitreous phase. The mullite composition is not stoichiometric and probably as temperature increases Si is partially replaced by Al, Fe and Ti in the structure. Nevertheless, with the increase of the firing temperature, the mullite composition is closer to the theoretical composition and also to that of natural mullites. Furthermore its crystal thickness increases with temperature up to 70 nm. The samples analysed in this study were taken from a shale outcrop

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The aim of this study is to analyze natural clinkers (= calcined clays by coal combustion) from a lower Cretaceous coal outcrop in Ariño (Teruel, NE Spain) in order to describe mineral and textural transformations produced during the spontaneous combustion of coal. To achieve this aim, samples were analyzed using X-ray diffraction and optical and electron microscopy. Spontaneous combustion resulted in the melting of the surrounding clays, with the generation of an Al–Si-rich vitreous phase. Subsequently, high-temperature phases crystallized from this vitreous phase. These new minerals are interesting due to their similarity with those formed during ceramic processes, used in the manufacture of stoneware and ceramic tiles, as well as in refractory ceramics, and with natural events such as metamorphic and igneous processes. The studied natural clinkers are composed of vitreous phase mullite, hematite, hercynite, cristobalite, quartz, pyroxenes, cordierite, gypsum, pyrite, and calcium oxides. A trend from hematite to hercynite composition indicates compositional variations at sample scale, which evidence d-spacing differences in hercynite and may be related to the Al and Fe content in hercynite depending on its texture. The mullite shows higher Si/Al ratio (1.21) than the theoretical composition (0.35), indicating that this mullite is more Si-rich. Three pyroxene-type compositions (diopside-type, ferrosilite-type, and a Ca–Al-rich pyroxene) were found. Both the mullite and the pyroxenes are nonstoichiometric.

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