Nicoletta Marinoni

Black limestone used in Lombard architecture

Abstract Black limestone samples from the quarries of Varenna (Lecco, I), Cene (Bergamo, I) and Riva di Solto (Bergamo, I) and widely used in Lombard architecture have been studied in terms of mineralogical, petrographic and chemical properties in order to provide a detailed characterisation and allow an unambiguous determination of their provenance. The inorganic and organic fractions have been separated from each other, and investigated using X-ray powder diffraction, atomic absorption, Hg-porosimetry, high performance liquid chromatography, gas chromatography, nuclear magnetic resonance and Fourier transform infrared spectroscopy. The occurrence of specific mineral phases, some binary chemical patterns (Fe/Mn, Zn/Sr, Zn/Co and Na/Cd) and the carbon chain relative molecular masses has proven to be useful markers to characterise unequivocally the materials studied.

Influence of aggregate mineralogy on alkali–silica reaction studied by X-ray powder diffraction and imaging techniques

Reliable assessment of the potential alkali reactivity of aggregate to develop deleterious alkali–silica reaction is essential for construction of durable concrete structures. The potential alkali reactivity of silicified limestone and two limestones has been investigated. Preliminary characterisation of aggregate was performed by optical and environmental scanning electron microscopy. X-ray powder diffraction peak profile analysis was used to predict the aggregates’ potential alkali reactivity. Samples were aged in accordance to the RILEM AAR-2 procedure and further characterised by means of optical and environmental scanning electron microscopy as well as by synchrotron X-ray microtomography, where quantitative analysis relative to damage due to the alkali–silica reaction (ASR) was performed by morphometric analysis of volume data. Results highlight that (1) the microstructural domain size and microstrain values extracted form XRPD line profile analysis seem to be good parameters for predicting the potential alkali reactivity of quartz in aggregate, and (2) the mineralogy of the aggregate influences the weathering products (i.e. aggregate dissolution, ASR gel growth and microcracking) due to ASR in cement-based materials.

The role of petrography on the thermal decomposition and burnability of limestones used in industrial cement clinker

The present research examines the influence of the petrographic features on the thermal decomposition and burnability of three limestones, the main raw materials for Portland cement-making. A detailed characterisation of the limestones has been performed by means of optical microscopy and X-Ray Powder Diffraction. The carbonate thermal decomposition was conducted under isothermal conditions by means of in situ High Temperature X-Ray Powder Diffraction and the heated samples were further investigated by Scanning Electron Microscopy. Three kiln feeds were then prepared and submitted to burning trials and the temperature of occurrence of the main clinker phases was investigated as well as the content of the uncombined CaO in the heated samples was determined by using the Franke method. The results attest that the microfabric, a combination of depositional and diagenetic features, drives the kinetics of the thermal decomposition of the selected limestones as well as it appears to influence the temperature of crystallisation of the main clinker phases and the uncombined CaO content in the final clinker. In particular, the limestone with the lowest micrite to sparite ratio (1) exhibits the lowest Apparent Activation Energy (Ea) value and the highest rate of calcination and (2) requires a lower temperature for observing the clinker phases crystallisation and has the lowest content of uncombined CaO in the final clinker, thus reflecting a high burnability of the limestone.

A compact and flexible induction furnace for in situ X-ray microradiograhy and computed microtomography at Elettra: design, characterization and first tests

A compact and versatile induction furnace for in situ high-resolution synchrotron and laboratory hard X-ray microradiography and computed microtomography is described. The furnace can operate from 773 to 1723 K. Its programmable controller enables the user to specify multiple heating and cooling ramp rates as well as variable dwell times at fixed temperatures allowing precise control of heating and cooling rates to within 5 K. The instrument can work under a controlled atmosphere. Thanks to the circular geometry of the induction coils, the heat is homogeneously distributed in the internal volume of the graphite cell (ca. 150 mm3) where the sample holder is located. The thermal gradient within the furnace is less than 5 K over a height of ca. 5 mm. This new furnace design is well suited to the study of melting and solidification processes in geomaterials, ceramics and several metallic alloys, allowing fast heating (tested up to 6.5 K s-1) and quenching (up to 21 K s-1) in order to freeze the sample microstructure and chemistry under high-temperature conditions. The sample can be held at high temperatures for several hours, which is essential to follow phenomena with relatively slow dynamics, such as crystallization processes in geomaterials. The utility of the furnace is demonstrated through a few examples of experimental applications performed at the Elettra synchrotron laboratory (Trieste, Italy).