In situ monitoring of corrosion processes by coupled micro-XRF/micro-XRD mapping to understand the degradation mechanisms of reinforcing bars in hydraulic binders from historic monuments

International audienceHistoric monuments have been partly built since antiquity with iron or steel reinforcements sealed in mortars or hydraulic binders. But the presence of chloride in the environment can weaken the structures due to the corrosion of these metallic parts, leading to the cracking of the binder. In this context, in order to better understand the first steps of these corrosion mechanisms a chemical cell was designed to operate in situ analyses of the phases precipitated when a chlorinated solution is introduced in the vicinity of the bar. The chemical and structural characterization (micro-XRF and micro-XRD respectively) was performed under synchrotron radiation at the SOLEIL-DiffAbs beamline. Moreover, complementary SEM-EDS analyses were carried out before and after the in situ cell experiment in order to determine the final localisation of the corrosion products inside the crack network. The results show that iron can spread up to 1 mm away from the metallic bar inside the pores of the binder after 44 h of corrosion. Moreover, in accordance with laboratory experiments conducted in solution in the presence of Fe2+ and Cl- ions the reaction pathways conduct to the successive formation of an intermediate Fe(ii)-Fe(iii) chlorinated green rust which transforms into ferric oxyhydroxides such as akaganeite or goethite depending on the local concentration of iron

Very first tests on SOLEIL regarding the Zn environment in pathological calcifications made of apatite determined by X-ray absorption spectroscopy

This very first report of a X-ray absorption spectroscopy experiment on Soleil is part of a more large long term study dedicated to ectopic calcifications. Such biological entities composed of various inorganic and/or organic compounds contain also trace elements. In the case of urinary calculi, different papers already published point out that these oligo elements may promote or inhibit crystal nucleation or growth of mineral or organic species involved. By using such tool specific to synchrotron radiation i.e. determine the local environment of oligoelements and thus their occupation site, we contribute to our understanding of the role of trace elements in ectopic calcifications

Diffraction techniques and vibrational spectroscopy opportunities to characterise bones

From a histological point of view, bones that allow body mobility and protection of internal organs consist not only of different organic and inorganic tissues but include vascular and nervous elements as well. Moreover, due to its ability to host different ions and cations, its mineral part represents an important reservoir, playing a key role in the metabolic activity of the organism. From a structural point of view, bones can be considered as a composite material displaying a hierarchical structure at different scales. At the nanometre scale, an organic part, i.e. collagen fibrils and an inorganic part, i.e. calcium phosphate nanocrystals are intimately mixed to assure particular mechanical properties

Investigating atmospheric corrosion behavior of carbon steel in coastal regions of Mauritius using Raman Spectroscopy

Low carbon steel was exposed at two sites in Mauritius, namely Port Louis and Belle Mare. The site at Port Louis is basically an industrial marine one whereas the one at Belle Mare is a purely marine site. Though the corrosion loss trend at both sites follow the power law, the corrosion loss at Port Louis was found to be higher than that at Belle Mare. This study has been performed to investigate the surface characteristics of the rust layers of the samples exposed at the two sites, through Raman spectroscopy and SEM, so as to get a better insight into the mechanism of the atmospheric corrosion process. For Port Louis, it was observed that there was not much change in the corrosion products in the rust layer over the 3 years period. The structure was less compact than that at Belle Mare with the presence of lepidocrocite and akaganeite as commonly observed corrosion products. The corrosion rate at Port Louis is, therefore, expected to follow the same trend over the long term. For Belle Mare, the corrosion products changed significantly after 3 years of exposure. Though lepidocrocite and akaganeite were observed on the surface after 0.2 years of exposure, magnetite was the most probable corrosion product in the more compact rust layer after 3 years of exposure. This compactness of the rust layer is expected to have reduced the corrosion rate as compared to that of Port Louis. Significant changes in the corrosion rate at Belle Mare are, therefore, expected over the medium and the long term

THESIC : Una plataforma flexible para la validation funcional de circuitos integrados

International audienceThis work aims at describing the main features of a system, the so-called THESIC tester, devoted to the functional validation of integrated circuits. This system, initially designed to set-up radiation test experiments of digital architectures, is composed of two main blocs: a motherboard for the interface with the user and the control of the circuit under test operation and a daughter board in which is implemented a suitable architecture around the circuit to be tested. The THESIC version presented in this paper was enhanced in order to significantly simplify the daughter board developments, whose architecture is implemented through an FPGA programmin

Synchrotron X-ray diffraction of bole layers from Portuguese gilded baroque retables

Studies based on a scientific approach to materials and techniques used in Portuguese gilded retables from the Baroque are very scarce and focus particularly on works with erudite features and on the characterization of the superficial gold leaf. The conservation and appearance of gilded surfaces, however, depended on the qualities of the clayey ground layer underneath, which is the bole. Colour and texture are closely related to its mineralogical composition. Boles were healing clays. Red to orange varieties could also be used for gilding, usually agglutinated with animal glue when the gold surface was meant to be burnished. Armenian was the name used to identify the best quality material. Microsamples collected from erudite and popular gilded retables, respectively belonging to the city of Oporto and its rural surroundings, were selected for elemental and mineralogical characterization. It was intended to shed light on the characteristics of boles used in Portuguese retables and to understand if there are any differences between materials used in works of distinct artistic quality. Elemental analysis was performed through SEM-EDS. SR-XRD was used for phase identification, performed with a six-circle diffractometer at the DIFFABS beamline of SOLEIL Synchrotron. Portuguese clay standards of identifiable composition and provenance were also analysed. The results suggest that boles are mainly kaolinitic, with variable amounts of illite and smectite. Gypsum was used as an extender. Although the proportions of the main clay minerals are similar in erudite and popular works, in Oporto homogeneity is clearly higher.info:eu-repo/semantics/publishedVersio

Synchrotron X-ray diffraction of bole layers from Portuguese gilded baroque retables

Studies based on a scientific approach to materials and techniques used in Portuguese gilded retables from the Baroque are very scarce and focus particularly on works with erudite features and on the characterization of the superficial gold leaf. The conservation and appearance of gilded surfaces, however, depended on the qualities of the clayey ground layer underneath, which is the bole. Colour and texture are closely related to its mineralogical composition. Boles were healing clays. Red to orange varieties could also be used for gilding, usually agglutinated with animal glue when the gold surface was meant to be burnished. Armenian was the name used to identify the best quality material. Microsamples collected from erudite and popular gilded retables, respectively belonging to the city of Oporto and its rural surroundings, were selected for elemental and mineralogical characterization. It was intended to shed light on the characteristics of boles used in Portuguese retables and to understand if there are any differences between materials used in works of distinct artistic quality. Elemental analysis was performed through SEM–EDS. SR-XRD was used for phase identification, performed with a six-circle diffractometer at the DIFFABS beamline of SOLEIL Synchrotron. Portuguese clay standards of identifiable composition and provenance were also analysed. The results suggest that boles are mainly kaolinitic, with variable amounts of illite and smectite. Gypsum was used as an extender. Although the proportions of the main clay minerals are similar in erudite and popular works, in Oporto homogeneity is clearly higher.info:eu-repo/semantics/publishedVersio

A marvel of medieval Indian metallurgy: Thanjavur's forge-welded iron cannon

In this article, metallurgical aspects of a 17th century forge-welded iron cannon at Thanjavur are addressed, including an analysis of manufacturing methodology based on careful observation of its constructional details. Microstructural examination of iron from the cannon reveals that the iron was extracted from ore by the direct process. Thus, the cannon was fabricated by forge welding and not by casting. Electrochemical polarization studies indicate that the corrosion rate of the cannon iron can be compared to that of 0.05% carbon mild steel under complete immersion conditions. However, the atmospheric corrosion resistance of the cannon is far superior to that of modern steel and can be attributed to the formation of an adherent protective passive fi lm. It is concluded that this cannon constitutes a marvel of medieval Indian metallurgical skill