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The kaolinite from Albian sedimentary deposits (Escucha and Utrillas Formations) of the Iberian Range (Spain) have been investigated. This research has shown the presence of different types of kaolinites (detrital and diagenetic) along with micaceous phases in these deposits. Detrital kaolinites show anhedral morphology, low crystallinity and a degree of ordering as well as the presence of interstratified smectite layers. They constitute the matrix of the claystones and siltstones and were probably formed as a consequence of intense weathering processes in the source area during the warm period of the early Cretaceous. Diagenetic kaolinites have been recognized in the sandstones and siltstones, with kaolinite growing between ‘expanded’ mica flakes and vermiform and euhedral kaolinite forming the matrix. They have euhedral morphologies, high crystallinity and a high degree of ordering. They grewin situas a response to incipient diagenesis by K-feldspar dissolution and/or organic acid-rich fluids derived from the maturation of organic matter in shales.

AB ST R ACT : This study uses transmission electron microscopy (TEM) and analytical electron microscopy (AEM) supported by X-ray diffraction (XRD) and scanning electron microscopy (SEM) to investigate the mineralogical and textural changes produced in carbonated clays by firing. Sample bars were prepared using raw clays composed of quartz, illite and carbonates with minor amounts of smectite, chlorite, feldspars and Fe oxides. The raw samples were then fired at temperatures of between 800 and 1050ºC. The XRD data show that increases in firing temperature result in dehydroxylation of clay minerals, carbonate decomposition and the formation of Ca-bearing silicates (e.g. gehlenite, wollastonite, pyroxenes and anorthite). The sizes of the Ca-silicate crystals make the use of the SEM inappropriate since they lie below the resolution threshold. However, TEM/AEM do provide the required textural and compositional characterization, revealing that there is a broad range of pyroxene compositions, some of which resemble fassaite, and that Ca/Mg ratios increase with temperature. The TEM also shows significant dehydroxylation and vitrification of the clay-rich matrix at T of~800ºC. Observed mineralogical and textural changes probably occurred in a system with a local disequilibrium much like small-scale, high-temperature metamorphic reactions (i.e. pyrometamorphism). The importance of these results is that they enable the selection of more appropriate raw clay composition and firing dynamics (temperature, firing duration and cooling rate) for both the brickmaking industry and brick conservation in the field of cultural heritage.

Abstraet--A sequence of interstratified illite-smectite (I-S) and illite in Paleozoic pelites and metapelites from the Iberian Range, Spain, was studied by X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The fine-grained matrix of diagenetic pelites is composed of I-S with sequences of illite-and smectite-like layers in a given sample. The Reichweite (R) values as determined by XRD and averaged over heterogenous I-S layer sequences increase with increasing grade, apparently continuously, in sharp contrast with TEM observations of other published sequences. Changes in I-S sequences along layers are rarely observed. In the higher-grade diagenetic pelites, I-S coexists with illite. Each I-S phase has a composition similar to that of illite, implying unique A1-Si distributions in contrast to smectite and muscovite, Selected area electron diffraction (SAED) patterns of I-S and illite are diagnostic of 1M a polytypism. Anchizonal metapelites consist of larger packets of wellcrystallized muscovite, with SAED patterns corresponding to a two-layer polytype.The continuous sequence of changes studied by TEM in I-S sequences and lateral transitions among these units is consistent with illitization by layer-by-layer replacement, although other processes are possible also. Replacement of individual layers probably occurs via fluids at reaction interfaces, in contrast to solid-state reactions, sensu strictu. The transition from the diagenetic to anchizonal rocks (transition in textures and formation of muscovite-2M~) occurred via dissolution/crystallization, however, presumably by tectonic stress. XRD and TEM data imply a consistent prograde trend in the sequence, the XRD data defining the average, long-range Reichweite ordering sequence, whereas the TEM data define the shortrange layer sequences.