16 research outputs found

    De Colorando Auro: Medieval colouring techniques researched using modern analytical techniques

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    The visual appearance of gold and gilding can be influenced in many ways, such as by changing the composition of the gold alloy or the nature of the gilded substrate. A less known medieval technique, reported in historical treatises, is the chemical treatment of the gilded surface itself, after application and burnishing of the gilding. We reporte here results regarding the study of the Holy Lady Shrine of Huy (13th c AD Mosan, Belgium) on which a possible artificial colouration of the gildings was detected. This led to many questions regarding applicable conservation-restoration treatments. Here is an overview of the results obtained, along with a discussion of the methodology that was developed to study this colouration process, also highlighting the necessary complementarity between laboratory and synchrotron-based analytical approaches. The 3-steps methodology proposed in this paper is generic for most cultural heritage problems where the application of ancient surface modification recipes is suspected but where the scarcity of the historical samples does not allow a direct study of such samples.L’aspect visuel de l’or et des dorures peut être modifié de diverses manières, notamment en changeant la composition de l’alliage ou la nature du support doré. Une technique médiévale moins connue, évoquée dans les traités anciens, consiste à provoquer une réaction chimique après application et brunissage de la dorure. Les recherches sur la châsse de Notre-Dame de Huy (art mosan du xiiie siècle) ont révélé une possible coloration artificielle des dorures. Cette découverte soulève de nombreuses questions quant aux traitements de conservation-restauration utilisables. Nous présentons ici un exposé sommaire des résultats obtenus ainsi qu’un compte rendu de la méthode mise au point pour étudier ce procédé de coloration, en soulignant la complémentarité indispensable entre les examens de laboratoire et l’analyse par rayonnement synchrotron. Dans les sciences du patrimoine culturel, cette méthode en trois temps concerne la plupart des situations où une recette ancienne semble avoir été employée pour modifier la surface, mais où la rareté des échantillons historiques ne permet pas l’étude directe de sous-échantillons

    AES analysis of nitride layers on steel with target factor analysis

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    Industrially nitrided steel samples are analysed with AES. The aim of this work is to optimize the quantification of nitrogen and to extract the chemical information hidden in the shape of the measured Auger peaks with Target Factor Analysis (TFA). To optimize the use of TFA, reference samples of pure components are necessary. These components are made in a laboratory reactor in which pure iron is nitrided. The resulting nitride layer is identified with X-Ray Diffraction (XRD). Afterwards their AES spectra are takers as input for the TFA of the industrial layers. In this paper, the preparation and the characterization of a γ′ -Fe4N standard is discussed, as well as the correction of the sensitivity factors used for the quantification of nitrogen. Finally, the application of TFA on art industrial nitride layer is discussed. Copyright © 2004 John Wiley & Sons, Ltd.SCOPUS: cp.jFLWINinfo:eu-repo/semantics/publishe

    Electroless deposited [Formula presented] coatings

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    An alkaline bath, initially designed for electroless deposition of amorphous [Formula presented] coatings, is used for plating of [Formula presented] by introduction of Ce3 + within the range 0.001–0.006 mol·dm− 3. A decrease in both deposition rate and phosphorus content in the coating in comparison with the typical for [Formula presented] is observed. By means of TEM, SAED and XRD nanocrystalline and amorphous structure is revealed. Applying scanning Auger electron spectroscopy, sputter etch profiles of constituent elements are composed. X-ray photoelectron spectroscopy spectra, taken inside the coating, demonstrate the chemical status of coating components. The transformations during annealing are studied by differential scanning calorimetry and magnetic properties. Increased thermal stability of electroless deposited [Formula presented] coatings is observed.SCOPUS: ar.jElectroless deposited Nisingle bondCesingle bondP coatingsinfo:eu-repo/semantics/publishe

    De Colorando Auro: Medieval colouring techniques researched using modern analytical techniques

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    REE and Hf distribution among mineral phases in the CV-CK clan : a way to explain present-day Hf isotopic variations in chondrites

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    Chondrites are among the most primitive objects in the Solar System and constitute the main building blocks of telluric planets. Among the radiochronometers currently used for dating geological events, Sm–Nd and Lu–Hf are both composed of refractory, lithophile element. They are thought to behave similarly as the parent elements (Sm and Lu) are generally less incompatible than the daughter elements (Nd and Hf) during geological processes. As such, their respective average isotopic compositions for the solar system should be well defined by the average of chondrites, called Chondritic Uniform Reservoir (CHUR). However, while the Sm–Nd isotopic system shows an actual spread of less than 4% in the average chondritic record, the Lu–Hf system shows a larger variation range of 28% [Bouvier A., Vervoort J. D. and Patchett P. J. (2008) The Lu–Hf and Sm–Nd isotopic composition of CHUR: Constraints from unequilibrated chondrites and implications for the bulk composition of terrestrial planets. Earth Planet. Sci. Lett.273, 48–57]. To better understand the contrast between Sm–Nd and Lu–Hf systems, the REE and Hf distribution among mineral phases during metamorphism of Karoonda (CK) and Vigarano-type (CV) carbonaceous chondrites has been examined. Mineral modes were determined from elemental mapping on a set of five CK chondrites (from types 3–6) and one CV3 chondrite. Trace-element patterns are obtained for the first time in all the chondrite-forming minerals of a given class (CK chondrites) as well as one CV3 sample. This study reveals that REE are distributed among both phosphates and silicates. Only 30–50% of Sm and Nd are stored in phosphates (at least in chondrites types 3–5); as such, they are not mobilized during early stages of metamorphism. The remaining fraction of Sm and Nd is distributed among the same mineral phases; these elements are therefore not decoupled during metamorphism. Of the whole-rock total of Lu, the fraction held in phosphate decreases significantly as the degree of metamorphism increases (30% for types 3 and 4, less than 5% in type 6). In contrast to Lu, Hf is mainly hosted by silicates with little contribution from phosphates throughout the CK metamorphic sequence. A significant part of Sm and Nd are stored in phosphates in types 3–5, and these elements behave similarly during CK chondrite metamorphism. That explains the robustness of the Sm/Nd ratios in chondrites through metamorphism, and the slight discrepancies observed in the present-day isotopic Nd values in chondrites. On the contrary, Lu and Hf are borne by several different minerals and consequently they are redistributed during metamorphism–induced recrystallization. The Lu/Hf ratios are therefore significantly disturbed during chondrites metamorphism, leading to the high discrepancies observed in present-day Hf isotopic values in chondrites

    Fatigue of Ti6Al4V structural health monitoring systems produced by selective laser melting

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    Selective laser melting (SLM) is an additive manufacturing (AM) process which is used for producing metallic components. Currently, the integrity of components produced by SLM is in need of improvement due to residual stresses and unknown fracture behavior. Titanium alloys produced by AM are capable candidates for applications in aerospace and industrial fields due to their fracture resistance, fatigue behavior and corrosion resistance. On the other hand, structural health monitoring (SHM) system technologies are promising and requested from the industry. SHM systems can monitor the integrity of a structure and during the last decades the research has primarily been influenced by bionic engineering. In that aspect a new philosophy for SHM has been developed: the so-called effective structural health monitoring (eSHM) system. The current system uses the design freedom provided by AM. The working principle of the system is based on crack detection by means of a network of capillaries that are integrated in a structure. The main objective of this research is to evaluate the functionality of Ti6Al4V produced by the SLM process in the novel SHM system and to confirm that the eSHM system can successfully detect cracks in SLM components. In this study four-point bending fatigue tests on Ti6Al4V SLM specimens with an integrated SHM system were conducted. Fractographic analysis was performed after the final failure, while finite element simulations were used in order to determine the stress distribution in the capillary region and on the component. It was proven that the SHM system does not influence the crack initiation behavior during fatigue. The results highlight the effectiveness of the eSHM on SLM components, which can potentially be used by industrial and aerospace applications

    In situ study of gas transport through Al(OH)3 gels during AC processing

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    In this work the nature of gas transport through different Al(OH)3 gels (smut) formed during the AC elec- trograining process is characterized. A new in situ approach that combines small angle X-ray scattering (SAXS) with the electrochemical response is used to show that gas transport through the smut is different with and without additives. We conclude that gas transport occurs, predominantly, through temporary passageways when no additives are used and through permanent pores with additives, indicating a dif- ference in the gel (smut) rheological properties in each case. Gas transport, through the smut, is therefore considered to be a phenomenon that depends on the electrolyte composition, which is expected to alter the gel properties. These changes in the gas transport away from the metal surface correlate with changes in the potential response of the system. The uniquely lower overpotential, associated with temporary pas- sageways results in an etched-like morphology, suggesting that the gas permeability of the surface gel is a factor that affects the final pit morphology.info:eu-repo/semantics/publishe

    Fatigue of Ti6Al4V structural health monitoring systems produced by Selective Laser Melting

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    Selective laser melting (SLM) is an additive manufacturing (AM) process which is used for producing metallic components. Currently, the integrity of components produced by SLM is in need of improvement due to residual stresses and unknown fracture behavior. Titanium alloys produced by AM are capable candidates for applications in aerospace and industrial fields due to their fracture resistance, fatigue behavior and corrosion resistance. On the other hand, structural health monitoring (SHM) system technologies are promising and requested from the industry. SHM systems can monitor the integrity of a structure and during the last decades the research has primarily been influenced by bionic engineering. In that aspect a new philosophy for SHM has been developed: the so-called effective structural health monitoring (eSHM) system. The current system uses the design freedom provided by AM. The working principle of the system is based on crack detection by means of a network of capillaries that are integrated in a structure. The main objective of this research is to evaluate the functionality of Ti6Al4V produced by the SLM process in the novel SHM system and to confirm that the eSHM system can successfully detect cracks in SLM components. In this study four-point bending fatigue tests on Ti6Al4V SLM specimens with an integrated SHM system were conducted. Fractographic analysis was performed after the final failure, while finite element simulations were used in order to determine the stress distribution in the capillary region and on the component. It was proven that the SHM system does not influence the crack initiation behavior during fatigue. The results highlight the effectiveness of the eSHM on SLM components, which can potentially be used by industrial and aerospace applications.status: publishe

    Photocatalytic TiO2 thin films synthesized by the post-discharge of an RF atmospheric plasma torch

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    Thin films of titanium oxide (TiO2) are synthesized at room temperature by the post-discharge of an RF atmospheric plasma torch supplied with argon and oxygen. Vapours of titanium tetraisopropoxide (TTIP) precursor are injected in the post-discharge by an argon flow rate bubbling in the liquid precursor. Without any external substrate heating, the coatings are amorphous and characterized by a thin film upon which agglomerates can be observed. The annealing of the coatings at 450 °C is efficient to (partially) crystallize the TiO2 since bands characteristic of the TiO2 anatase structure are observed in Raman spectra. The films are super-hydrophilic and present excellent photocatalytic activity; two properties of particular interest for self-cleaning applications. Nevertheless, annealed coating presents a higher photocatalytic activity.SCOPUS: ar.jinfo:eu-repo/semantics/publishe
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