Table 1 - uploaded by Trinitat Pradell
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Composition corresponding to the glaze and to the paste for the samples studied. The data is given in wt%
Source publication
The production of glass represented an important technological achievement, and it was the starting point for the invention of a large variety of materials, produced by processes involving melting, partial or total, and precipitation of new crystalline compounds during cooling. In particular, those crystallites built-in the glaze due to partial or...
Contexts in source publication
Context 1
... chemical analyses of the glassy matrix and pastes measured on the polished cross section of the glaze are shown in Table 1. ...
Context 2
... analyses confirm the alkaline nature of inter- stitial glass and glaze, see Table 1. The alkaline content is relatively high in the interstitial glaze (10.8 ...
Context 3
... glazes are tin-opacified and relatively lead rich, about 20 wt% PbO, see Table 1. Micro-XRD analysis of the glaze (Fig. 2b) shows the presence of cassiterite (SnO 2 , JPDF file 77-0452) and pyroxenes crystals of diopside type (CaMgSi 2 O 6 , JPDF file 71-1494) and does not contain cristobalite nor quartz inclusions. ...
Context 4
... has a yellow greenish lustre paint applied over a translucent glaze on a creamy coloured ceramic body with a buff colour and a sandy consistency of small grain size and corresponds with the calcareous fine grain pastes (14% CaO) [22] from this period. The glaze has a high lead content (34 wt% PbO), see Table 1, containing some bubbles, a few quartz, cristo- balite and cassiterite particles. The lack of a reaction layer (Fig. 4a) suggests that the ceramic bodies were fired be- fore the application of the glaze mixture. ...
Citations
... The formation of lead-potassium feldspars (Figure 11.9), with low lead content, is typical for gla es deposited on a potassium-rich clay substrate (Molera et al. 1993Pradell et al. 2010. Lead sanidine crystals were frequently identified in lead gla es (Molera et al. 1993Pradell et al. 2010Coentro et al. 2017) they seem to occur for Na-poor clays (Pradell et al. 2010) and, occasionally, by epitaxial growth on potash feldspar crystals (Molera et al. 1993). ...
... The formation of lead-potassium feldspars (Figure 11.9), with low lead content, is typical for gla es deposited on a potassium-rich clay substrate (Molera et al. 1993Pradell et al. 2010. Lead sanidine crystals were frequently identified in lead gla es (Molera et al. 1993Pradell et al. 2010Coentro et al. 2017) they seem to occur for Na-poor clays (Pradell et al. 2010) and, occasionally, by epitaxial growth on potash feldspar crystals (Molera et al. 1993). Sanidine is a high-temperature feldspar of nominal composition KAlSi 3 8 , with a maximal degree of Si Al disorder (Si and Al are randomly distributed on tetrahedral sites Brown and Parsons 1989). ...
... The formation of lead-potassium feldspars (Figure 11.9), with low lead content, is typical for gla es deposited on a potassium-rich clay substrate (Molera et al. 1993Pradell et al. 2010. Lead sanidine crystals were frequently identified in lead gla es (Molera et al. 1993Pradell et al. 2010Coentro et al. 2017) they seem to occur for Na-poor clays (Pradell et al. 2010) and, occasionally, by epitaxial growth on potash feldspar crystals (Molera et al. 1993). Sanidine is a high-temperature feldspar of nominal composition KAlSi 3 8 , with a maximal degree of Si Al disorder (Si and Al are randomly distributed on tetrahedral sites Brown and Parsons 1989). ...
A vitreous coating on ceramic has several functions: a practical one, by waterproofing and protecting the earthenware object, but also an esthetic and symbolic one. The extent and the nature of the interface connecting the two materials - fired clay of the body and glassy material of the decoration - play an essential role in the final composition of the glaze and many physicochemical properties of the finished object. Relying on the pioneering and very detailed works of Molera et al. (2001), Walton (2004), Ben Amara (2002) and the recent works of Roisine (2018) and Godet et al. (2019), this chapter proposes a review of the state of knowledge for lead-rich glazes.
... Finally, individual CAY030 differs from F3 because of vaterite (Fig. 8b), a rare calcium carbonate polymorph that has been previously reported in early modern ceramics (Iñañez 2007;Dias et al. 2012) and that could be present in individuals OLL008 and CAY027 (F1). The presence of vaterite is of a secondary origin from a Ca-rich wet environment (Pradell et al. 2010). ...
The archaeological knowledge of the material culture in the city of Córdoba (Andalusia, Spain) during the late medieval and early modern periods is very scarce. Urban rescue excavations and archive sources evidence that the so-called Barrio de las Ollerías (potters’ quarter) was the main ceramic production area from the early medieval period until the end of the early modern period. Nevertheless, there is a total lack of archaeological and archaeometric studies since research has traditionally focused on Seville city and other production centres closer to the Atlantic Coast. However, archaeological and archaeometric studies concerning Islamic pottery have increased in Córdoba in the last years, although there is a lack of studies on the late medieval and early modern ceramic production. This article aims to contribute to filling this gap through an exhaustive study of the ceramic production of Córdoba in this period. As a first objective, studying the ceramics recovered from the workshops will enable us to define the chemical reference groups (RG). The second step will be the approach to the technology used by the potters for the elaboration of the different products. With these objectives in mind, 120 individuals have been chemically characterised using x-ray fluorescence analysis (XRF) and mineralogically through x-ray diffraction analysis (XRD). The sample includes tin-lead glazed vessels, coarse and cooking ware vessels, and storage and transport jars dated from the fifteenth to the eighteenth centuries.
... La formation des feldspaths plomb-potassium (figure 11.9), pauvres en plomb, est typique des glaçures posées sur substrat argileux riche en potassium (Molera et al. 1993 ;Pradell et al. 2010). Des cristaux de sanidine plombifère ont été fréquemment identifiés dans les glaçures au plomb (Molera et al. 1993 ;Pradell et al. 2010 ;Coentro et al. 2017) ; ils semblent survenir pour des argiles pauvres en Na (Pradell et al. 2010) et, occasionnellement, par croissance épitaxiale sur des cristaux de feldspaths potassiques (Molera et al. 1993). ...
... La formation des feldspaths plomb-potassium (figure 11.9), pauvres en plomb, est typique des glaçures posées sur substrat argileux riche en potassium (Molera et al. 1993 ;Pradell et al. 2010). Des cristaux de sanidine plombifère ont été fréquemment identifiés dans les glaçures au plomb (Molera et al. 1993 ;Pradell et al. 2010 ;Coentro et al. 2017) ; ils semblent survenir pour des argiles pauvres en Na (Pradell et al. 2010) et, occasionnellement, par croissance épitaxiale sur des cristaux de feldspaths potassiques (Molera et al. 1993). La sanidine est un feldspath de composition nominale KAlSi 3 O 8 , ayant un degré maximal de désordre Si/Al (Si et Al sont distribués aléatoirement sur les sites tétraédriques (Brown et Parsons 1989)) et se formant à haute température. ...
... La formation des feldspaths plomb-potassium (figure 11.9), pauvres en plomb, est typique des glaçures posées sur substrat argileux riche en potassium (Molera et al. 1993 ;Pradell et al. 2010). Des cristaux de sanidine plombifère ont été fréquemment identifiés dans les glaçures au plomb (Molera et al. 1993 ;Pradell et al. 2010 ;Coentro et al. 2017) ; ils semblent survenir pour des argiles pauvres en Na (Pradell et al. 2010) et, occasionnellement, par croissance épitaxiale sur des cristaux de feldspaths potassiques (Molera et al. 1993). La sanidine est un feldspath de composition nominale KAlSi 3 O 8 , ayant un degré maximal de désordre Si/Al (Si et Al sont distribués aléatoirement sur les sites tétraédriques (Brown et Parsons 1989)) et se formant à haute température. ...
Bien que le développement du cristal au plomb constitue une étape majeure dans l’histoire du verre à la fin du XVIIe siècle, la présence de plomb dans des matrices vitreuses (verres et glaçures) est beaucoup plus ancienne, son usage date du second millénaire avant notre ère.Le plomb dans les matériaux vitreux du patrimoine retrace l’histoire de ces savoir-faire et s’intéresse également aux développements les plus récents en sciences des matériaux concernant le rôle joué par le plomb dans les propriétés des verres, dont la coloration. Il développe la compréhension des processus d’altération et les notions de durabilité des verres au plomb. Il étudie également les problèmes de santé publique et les normes actuellement recommandées pour l’utilisation du plomb dans les verres industriels.Pluridisciplinaire, cet ouvrage s’adresse à un large public : historiens de l’art et des techniques, conservateurs de musée, restaurateurs, spécialistes des matériaux, industriels ou ingénieurs.
... A cross-section of a ceramic tile sample was prepared to identify the glaze interaction region with the body besides the glaze layer thickness (Pradel et al. 2010;Moussa and Ali, 2013). The prepared cross-section was examined using SEM to identify the varied thickness of the glaze layer. ...
The Sapil (public fountain) and Kuttab (school) of Mustafa Sinan are important monuments dating back to the Ottoman Era (1630 AD). The main façade of the Sapil in the southeastern side on the Soq al-Silah Street has a set of ceramic tiles with floral decorations, but heavily deteriorated from environmental factors. In fact, the tiles suffered severe deterioration, causing some deterioration phenomena, such as crazing and large, macro cracks, peeling of the glaze layer, broken ceramic tiles and accumulated dust and soot on the surface, resulting in the deformation and obliteration of the decorations. The present research paper is a characterization study (chemical composition and mineralogical structure of the body and the glaze layer) to determine their deterioration aspects. USB digital microscope, X-Ray Diffrac-tion, and SEM-EDX were used to study ten various samples. The results of tiles analysis showed the use of local clay mixed with a small amount of lime. The firing temperature of these tiles was around 900-1000 ºC according to the presence of diopside. The mortar of the installation of the ceramic tiles was composed of a mixture of gypsum, lime, and sand. It was determined that the alkaline and lead oxides were the main components of the glaze layer, with rising lead oxide in all samples. It was also seen that the white glaze color was obtained with calcium, whereas the cobalt oxide was used for dark blue. At the same time, the copper oxide was used for light blue and green color. Iron oxide with manganese was used to get the coral red glaze. This helped to choose compatible materials for their future restoration.
... The small beam spot, relatively high energy and high flux of the beamline make it suitable for the measurement of archaeological materials in transmission even when the absorption of the sample is high. 33,34,40 However, in the current study, the analysed sample containing arsenic-bearing phases was too thick for the transmission measurement, and it was carried out in reflection geometry. In this regard, the sample was measured in reflection mode at different incidence angles (omega X) so that: ...
New excavations at Espidej at the Kerman province of the Halil Basin corridor in Iran offer a unique opportunity to re‐consider the 3th millennium BC (i.e. Bronze Age) metallurgical practices related particularly to arsenical copper (Cu‐As) alloying and to explore arsenic bearing raw materials. This paper presents results of optical microscopy and environmental scanning electron microscopy (ESEM) on a selected group of copper‐based artefacts from Espidej. Additionally, we have benefited from synchrotron light for further investigations on a dagger sample. The scientific examinations on metal corpora adds new information regarding the microchemistry and production techniques of metals of the south‐eastern cultural zone of Iran. Synchrotron micro X‐ray diffraction (SR‐μXRD) data of the sample demonstrates traces of arsenic‐bearing minerals in the corrosion products indicative of types of ores used in alloying processes. Preliminary research on copper ores indicates possible extraction of local ore deposits which were outcropped along the south east Makran orogeny zone of Iran. This area is part of hydrothermal mineralization zone consisting of arsenopyrite (FeAsS), sinnerite (Cu6As4S9), bornite (Cu5FeS4) and algodonite (Cu6As). Noticeable arsenic bearing phases within the metallic core of the sample were frequently characterised as sinnerite and algodonite.
... Being heterogenous materials, the analysis of ceramics can benefit from the combination of different SR-based X-ray methods with micrometric or sub-micrometric spatial resolutions. For example, µ XRF can be combined with micro-X-ray diffraction (µ XRD) for the determination of crystalline phases in both the ceramic body and decorative layers or nano-XRD for single crystal studies even in not-crystalline matrix, such as in glazes [24][25][26]. µ XRF can be also coupled with µ -or nano-XANES, enabling the determination and even the distribution of the valence state of an element [27]. Usually, this method requires the preliminary acquisition of a µ XRF map for the selection of areas of interest. ...
Synchrotron X-ray µ- and nano-probes are increasingly affirming their relevance in cultural heritage applications, especially in material characterization of tiny and complex micro-samples which are typical from archaeological and artistic artifacts. For such purposes, synchrotron radiation facilities are tailoring and optimizing beamlines and set-ups for CH, taking also advantages from the challenges offered by the third-generation radiation sources. In ancient ceramics studies, relevant information for the identification of production centers and manufacture technology can be obtained in a non-invasive and non-destructive way at the micro-sample level by combining different SR based methods. However, the selection of appropriate beamlines, techniques and set-ups are critical for the success of the experiments. Fine and varnished wares (e.g., Attic and western-Greek colonial products) are an excellent case study for exploring challenges offered by synchrotron X-ray microprobes optimized to collect microchemical and phase-distribution maps. The determination of provenance and/or technological tracers is relevant in correctly classifying productions, often based only on ceramic paste, gloss macroscopic features or style. In addition, when these vessels are preserved in Museums as masterpieces or intact pieces the application of non-invasive approach at the micro sample is strictly required. Well-designed synchrotron µXRF and µXANES mapping experiments are able providing relevant clues for discriminating workshops and exploring technological aspects, which are fundamental in answering the current archaeological questions on varnished Greek or western-Greek colonial products.
... Differences in morphology could be explained also in conjunction with the crosssection SEM images of the glazed samples ( Figure 4). The bubbles formation into the glaze mass could be explained, according to [48], considering the following gas sources: (i) evaporation of the volatile substances contained by the enamel dispersion such as water and organic solvents; (ii) release of the gas trapped in the pores of the support material (MDF) during melting of the glaze; (iii) release of the dissolved gas from the enamel dispersion during the heating process; (iv) release of the gaseous products obtained by additives degradation. ...
... The bubbles formation into the glaze mass could be explained, according to [48], considering the following gas sources: (i) evaporation of the volatile substances contained by the enamel dispersion such as water and organic solvents; (ii) release of the gas trapped in the pores of the support material (MDF) during melting of the glaze; (iii) release of the dissolved gas from the enamel dispersion during the heating process; (iv) release of the gaseous products obtained by additives degradation. ...
Macro defect free (MDF) cements are polymer-cement composites characterized by high biaxial flexural strength compared to traditional concrete, having as a drawback a low water resistance. Glazing these composite materials with an inorganic enamel containing TiO2 nano-particles has led to a high water-stable material with advanced photocatalytic properties. Classic glazing by thermal treatment of samples, at 1050 °C, requires energy consumption and long-time performing. The purpose of this paper is to test the use of solar radiation as a source of energy in the glazing process. A vertical axis solar furnace has been used, from PROMES-CNRS Solar Laboratory, Font-Romeu Odeillo, France, and it has been observed that a uniform appearance of the glaze coating has been achieved; it shows high scratch resistance, meaning a good hardness and adhesion to the substrate. The obtained film was also characterized by SEM, EDS and XRD, aiming to evidence the coat morphology, the TiO2 distribution and its crystallinity alteration, when compared to the samples obtained by classic thermal treatment. The conclusion of the paper is that using solar radiation in the MDF cement glazing process is a promising approach for obtaining multifunctional materials.
... [11] . 因而会聚后X射线束照射在 表面不平整样品上时, X射线衍射峰位不会因样品 表面存在的空隙、弯曲度或不平整而发生偏移, 从 而能极大地提高X射线衍射分析的强度、准确性 和灵敏度 [12] . ...
In order to realize micron scale to millimeter scale phase structure analysis, as well as accurate phase structure analysis of surface uneven samples, X-ray diffractometer named Hawk-II, which can adaptively adjust the diameter of irradiated X-ray beam spot according to the diameter of internal tangential circle at the measured point, is developed by combining X-ray diffraction technology, CCD camera imaging technology and slightly-focusing ploycapillary X-ray control technology. The X-ray source system, six-dimensional linkage motion system, CCD camera, detection system and control system based on LabVIEW are the main components of the Hawk-II. Compared with the 3°–5° divergence of the conventional X-ray source, the divergence of the X-ray emitted by the slightly-focusing polycapillary X-ray optics is only about 0.15° and also the intensity within the beam spot range is dozens of times stronger. Therefore, the shift of peak position will not appear due to the pores, curvature or uneven surface of the sample, when Hawk-II is used to analyze the samples with irregular surface. The diffraction pattern of the uneven Ren Min Bi five-cent coin are collected in the Hawk-II and PANalytical X-Pert Pro MPD conventional X-ray diffractometer respectively. By comparing the analysis results, it is found that the diffraction peaks measured by the X-Pert Pro MPD are shifted seriously, with a maximum deviation angle of 0.52°. While the diffraction peaks detected by the Hawk-II are basically consistent with the data from the standard PDF card, which verifies the advantages of the analysis of irregular samples by the Hawk-II. In order to explore the difference between different beam spots used for analysis at the same point, red and green porcelain fired in Qing dynasty and GaAs-based Cu and Fe plated films are analyzed by the Hawk-II. It is found that when the samples are relatively uniform, the intensities of diffraction peaks of different beam spots are relatively close, while when the samples are not uniform, the diffraction peaks vary greatly. Especially, some microcrystalline phases can be detected only with large beam spots. In addition, to verify the adaptive functionality of the Hawk-II, a bronze from the Western Han Dynasty, with different rust spots on it, is tested. It is found that the Hawk-II can adjust the beam spot size according to the different corrosion points, making the irradiation area coincide with the area to be analysed and the phase structure detected more accurately. Therefore, the Hawk-II is a general purpose X-ray diffractometer, which has the analytical capability from micron scale to millimeter scale and the energy dispersive X-ray fluorescence analysis function. Moreover, it has the advantages of the accurate analysis of irregular samples, fast detection speed, simple operation, etc. Based on the above analysis, the Hawk-II will be widely used in different fields.
... The microbeam of synchrotron or of rotating anode X-ray sources can be used for local analysis (µXRF or µXRF). [80][81][82][83][84][85] Transmission electron microscopy (TEM), in particular coupled with focused ion beam (FIB) for the final preparation of the sample, is the unique technique to study microstructure at nanometer and sub-nanometer scale. However, it is expensive and time-consuming to study many samples and therefore the representativeness of the measurements is not obvious. ...
... Only transmission electron microscopy (TEM) provides topological information at submicron scale. 52,[82][83][84][85][86][87][88][89] Fig. 7 shows some examples. Lustre decor arises from the controlled dispersion of metal nanoparticles in the glaze close to its surface. ...
Much like weapons, vessels made from glasses and ceramics have long been held as objects of very high technology. Ceramic technology mastery is even at the foundation of metallurgy. In producing glass, potteries and enamelled metals, three critical, and energy intensive steps areneeded: obtaining fine powder, firing, and building appropriate kilns. Control of the colour also requires advanced physical and chemical knowledge. Indeed, if ceramic production is somewhat the art of forming a heterogeneous matter (only some components melt), glass or enamel production requires the object to pass through a homogeneous liquid state to obtain the desired microstructure and properties. This chapter presents the different destructive, non-destructive and non-invasive analytical methods that can be carried out in laboratory, on shards or sampling with fixed 'big' instruments, or on site (museums, reserves, etc.) with mobile setups. After a brief overview of the history of pottery, the implications of the processes involved (grinding, shaping, sintering, enamelling, decoration) on micro-and nano-structures (formation / decomposition temperature, kinetic / phase rules, sintering) is given. The emphasis is given to information that can be obtained by XRF and Raman mobile non-invasive measurements. Examples illustrating how these studies help to document technology exchanges and exchange routes are also given.
... The microbeam of synchrotron or of rotating anode X-ray sources can be used for local analysis (mXRF or mXRF). [80][81][82][83][84][85] Transmission electron microscopy (TEM), in particular coupled with focused ion beam (FIB) for the final preparation of the sample, is a unique technique to study microstructure at nanometre and sub-nanometre scale. However, it is expensive and timeconsuming to study many samples and therefore the representativeness of the measurements is not obvious. ...
... Only transmission electron microscopy (TEM) provides topological information at the submicron scale. 52,[82][83][84][85][86][87][88][89] Figure 7.7 shows some examples. Lustre decor arises from the controlled dispersion of metal nanoparticles in the glaze close to its surface. ...
