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Journal of Thermal Analysis and Calorimetry
Authors: M. Franquelo, M. Robador, V. Ramírez-Valle, A. Durán, M. Jiménez de Haro, and J. Pérez-Rodríguez

Abstract  

Roman ceramics of two hydraulic mortars used to build the pond and water channel of Mithraeum house from Mérida (Spain) have been studied. The sizes of the ceramic fragments found were different in both of the samples studied, showing different behaviour in the reactions with the lime. The X-ray diffraction of the ceramic shows the presence of quartz, mica (biotite), anorthite and hematite accompanied by amorphous phase, being observed scarce vitrification. The presence of mica confirms a firing temperature for manufacturing the ceramic below 900°C. In one of the ceramics studied, X-ray diffraction did not show calcite. However, in the FTIR appear bands that could be assigned to carbonates absorptions and likewise, carbonates were identified in the DTA-TG curves. Ca and small quantities of Si and Al were also identified by SEM-EDX on the surface of the pores that could be due to an amorphous phase formed in the reaction of lime with the Si and Al of the ceramic. On the other hand, in other ceramic samples carbonates (about 10%) were detected. The carbonates have been found filling the pores, sometimes accompanied by a new calcium-aluminium-silicate phase produced by the reaction between the lime and the amorphous phase of the ceramic. The carbonates and the new phases formed inside the pores are responsible for the decrease of the porosity and for the formation of new phases during the heating of the ceramics.

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Summary  

The differences on the thermal behaviour (DTG-DTA) of antigorite sample measured before and after sonication have been studied. Sonication treatment produces negligible changes in the structure of the material but substantial textural modifications. These modifications produce changes in the thermal behaviour of antigorite sample. Thus, it has been observed a decrease in the dehydroxylation temperature as measured by DTG and DTA effects. For sonication treatments longer than 20 h, two new effects of dehydroxylation are observed, the intensity of these two new effects increases with the sonication time showing a modification in the release of structural OH. It has been also observed that the formation of forsterite takes place simultaneously with the dehydroxylation of the antigorite. The high temperature exothermic effect is due to the recrystallization of forsterite and not to the formation of forsterite as traditionally assumed. Modifications in the thermal dehydroxylation of antigorite observed in this study are related to the pronounced decrease in particle size obtained by sonication.

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Journal of Thermal Analysis and Calorimetry
Authors: V. Balek, L. Pérez-Maqueda, J. Poyato, Z. Černý, V. Ramírez-Valle, I. Buntseva, and J. Pérez-Rodríguez

Abstract  

The effect of grinding on thermal behavior of pyrophyllite and talc as commonly used ceramic clay minerals was investigated by DTA, TG, emanation thermal analysis (ETA), B.E.T. surface area (s.a.) measurements, X-ray diffraction (XRD) and scanning electron microscopy (SEM). A vibratory mill was used in this study, grinding time was 5 min. It was found that the grinding caused an increase in surface area and a grain size reduction of the samples. From TG and DTA results it followed that grinding caused a decrease of the temperature at which the structure bound OH groups released. The formation of high temperature phases was enhanced with the ground samples. For the ground talc sample the crystallization of non-crystalline phase into orthorhombic enstatite was observed in the range of 800°C. For ground pyrophyllite a certain agglomeration of grains was observed in the range above 950°C. Moreover, for both clays the ETA characterized a closing up of subsurface irregularities caused by grinding as a decrease of the emanation rate in the range 250–400°C. The comparison of thermal analysis results with the results of other methods made it possible to better understand the effect of grinding on the ceramic clays.

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Journal of Thermal Analysis and Calorimetry
Authors: V. Ramírez-Valle, M. Jiménez de Haro, M. Avilés, L. Pérez-Maqueda, A. Durán, J. Pascual, and J. Pérez-Rodríguez

Abstract  

Static and dynamic heating of vermiculite samples from Santa Olalla, Huelva, Spain, saturated with different cations, i.e. Na+, Cs+, NH4 +, Mg2+, Ca2+, Ba2+ and Al3+, have been studied. The characterization of the phases formed during heating has been carried out by X-ray diffraction. The phases formed depend on the cation present in the interlamellar position and the heating process. The phases identified in the vermiculite samples saturated with different cations and heated at different temperatures are the following: enstatite, forsterite, spinel, cordierite, anorthite, pollucite, nepheline, coesite, celsian and others various mixed silicates; also some dehydrated and amorphous phases have been observed. On static heating, at the maximum temperature reached in this work, the phases formed appear mixed with a glassy phase.

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Journal of Thermal Analysis and Calorimetry
Authors: L. Pérez-Maqueda, V. Balek, J. Poyato, J. Šubrt, M. Beneŝ, V. Ramírez-Valle, I. Buntseva, I. Beckman, and J. Pérez-Rodríguez

Abstract  

Thermal behavior of talc samples (from locality Puebla de Lillo, Spain) were characterized by emanation thermal analysis (ETA), DTA and TG. The ETA, based on the measurement of radon release rate from samples, revealed a closing up of surface micro-cracks and annealing of microstructure irregularities of the talc samples on heating in the range 200–500°C. For ground talc sample a crystallization of non-crystalline phase formed by grinding, into orthorhombic enstatite was characterized as a decrease of radon mobility in the range 785–825°C and by a DTA exothermal effect with the maximum at 830°C. ETA results characterized the microstructure development of the talc samples on heating and served to evaluate their radon mobility and transport properties on heating and cooling. Transport properties of the talc samples were evaluated by using ETA experimental data measured during heating to 600 and 1300°C, respectively, and subsequent cooling to room temperature.

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