We demonstrate the utility of Raman spectroscopy as a technique for the identification of ancient glasses and enamel coatings of ceramics. As for any silicate glasses, the addition of network modifiers breaks the Si–O linkages and modifies the degree of polymerization and hence the relative intensity of the Si–O bending and stretching modes. We demonstrate empirically that the ratio of these envelopes is well correlated to the glass structure and to the firing technology used. Spectral Qn components assigned to isolated and connected SiO4 vibrational units allow more precise analysis. Selected porcelains, faiences, potteries and glasses representative of the different Asian, Islamic and European production technologies were studied. Modern porcelain enamels are used as compositional references.

https://hal.archives-ouvertes.fr/hal-00124997/document

Polymerization degree and Raman identification of ancient glasses used for jewelry, ceramic enamels and mosaics

The coloring efficiency in different ceramic glazes of the classical Co olivine blue pigment (Co2SiO4) was compared with those obtained with a Co-doped willemite (Co0.05Zn1.95SiO4), and with a magnesium-doped Co-Al spinel (Mg0.2Co0.8Al2O4). The fired pigments and enameled samples were characterized by XRD, UV-VIS-NIR spectroscopy, CIE-L*a*b* color-measurements, and by SEM/EDX. The Co-olivine and Co-willemite pigments dissolved to a higher extent in the molten glazes than the Co–Al spinel. The darker blue color of the Co-olivine probed to be mostly due to Co2+ ions incorporated in the glassy matrix. The Co-willemite composition (which only contained a 1.3 Co wt.%) developed the bluest color hue of all pigments in both double and single firing glazes, while the magnesium-doped Co–Al spinel was found the most appropriate blue pigment in the bulk coloration of fast-fired porcelainized stoneware.

Colour analysis of some cobalt-based blue pigments

Two palettes, characteristic of the production of the Sevres Factory (Manufacture Nationale de Sevres), and representative of ancient glazing techniques, were studied. One was made with coloured glazes/enamels on Bisque (1050 °C) and the other one was composed of Moufle (880 °C) painting colours. Spectra specific to the white (opacifiers), yellow (including Naples yellow), green, pink, ‘brown–red’ and black coatings/paintings were considered. Emphasis was placed on the different Raman peaks arising from coloured coatings specific to ancient artefacts: greens obtained with dissolved Cu ions or from chromium pigments (Victoria green garnets), Naples yellows (Pb2Sb2O7 pyrochlore), green and black spinels and pink sphene. Attention was paid to the effect of pigment grain size on the Raman spectrum. To illustrate the capability of the method, we analysed some old artefacts from the eighteenth and nineteenth centuries. Copyright © 2001 John Wiley & Sons, Ltd.

Differentiation of antique ceramics from the Raman spectra of their coloured glazes and paintings

The utility of Raman spectroscopy as a non-destructive technique for the characterization of glassy (alumino)silicates (modern or ancient glazes and glasses) is demonstrated. The addition of fluxing ions breaks the Si–O linkages and the degree of (de)polymerization determines the relative intensity of the Si–O bending and stretching modes and hence the degree of polymerization could be classified. The analysis can be used to predict the processing temperature of glasses. Bending (Q′n) and stretching (Qn) spectral components assigned to isolated (Q0 or SiO4), and more or less connected SiO4 vibrational units with one, two three/four bridging oxygen allow more precise analysis. The method is applied to reference modern porcelain glazes and selected ancient ceramic glazes and glasses, representative of the different production technologies used in the Asian, Islamic, and European worlds from Roman Empire to 19th century.

Non-Destructive Determination of the Structure and Composition of Glazes by Raman Spectroscopy

On-site Raman analyses were performed at the Musee National de Ceramique, Sevres, France, on rare Iznik (former Nicaea) pottery produced from ∼1480 to ∼1620. A comparison was made with a series of shards. The town of production of these potteries was highly disputed in the 1980s and many questions still remain. The potential of glaze on-site analyses as a classification/dating tool was evaluated. The structure of the silicate glaze does not change with the sample (index of polymerization ∼0.5–0.8, indicating a lead silicate composition); characteristic SiO stretching mode doublet at ∼985 and 1030–1050 cm−1. By contrast, the corresponding signature of most of the ‘Kutahya’ wares peaks at ∼1070–1090 cm−1. The lowest index is measured for a brilliant overglazed red bole, according to a lower temperature of (post)firing. The different crystalline phases identified in the glaze are α-quartz, haematite, spinel, cassiterite, uvarovite garnet and zircon. White colour arises from α-quartz slip in most samples studied. Cassiterite (SnO2) opacifier is only present in some early blue-and-white ceramics (Master of the Knots and Baba Nakkas style, ∼1510–1530) and we do not have other evidence of its intentional use as an opacifier. Intentional addition of tin oxide is likely for colour lightening in some red, blue and in clear green boles. At least two types of red glazes and two types of Cr-containing green pigments are evidenced. Copyright © 2004 John Wiley & Sons, Ltd.

On Site Raman Analysis of Iznik Pottery Glazes and Pigments

Machine generated contents note: PART I. -- Introduction -- 1 Introduction -- 2 The Nature of Glass -- PART II. -- Chemistry of Glazes and Enamels -- 3 Formulation of Glazes -- 3.1 Method of Presentation. -- 3.2 Role of the Oxides, -- 3.3 Leadless Gloss Glazes -- 3.4 Lead Glazes -- 3.5 Opaque Glazes -- 3.6 Satin and Matte Glazes -- 3.7 Glazes for Special Effects. -- 4 Formulation of Enamels -- 4.1 Adherence to a Metal -- 4.2 Ground Coat Enamels -- 4.3 Cover Coat Enamels -- 5 Raw Materials for Ceramic Coatings -- 5.1 Sources of the Oxides -- 5.2 Raw Materials to Avoid -- 5.3 Frits. -- 5.4 Kinetic Effects in Glazing -- 6 Batch Calculation -- 6.1 Batch to Oxide -- 6.2 The Role of Judgment -- 6.3 Oxide to Batch -- 6.4 Computer Programs -- 7 Mill Additives and Slip Rheology. -- 7.1 Binders -- 7.2 Deflocculants -- 7.3 Flocculants -- 7.4 Suspending Agents -- 7.5 Other Additives -- 7.6 Slip Rheology -- 8 Color in Glazes and Enamels -- 8.1 What is Color? -- 8.2 Color Spaces --^

Glazes and glass coatings

The Relative Stability of Ceramic Pigments

Analyzing the Color of Reddish Glazes

Formulation of Leadless Glazes

Controlling the Gloss of Leadless Glazes

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