Historical glass-based objects undergo, since the time of their manufacture, different degradation phenomena that are related to their composition and to the environment to which they were exposed. Three-dimensional (3D) structural and chemical characterization of the degradation layers is important to select the most adequate conservation strategies for glass objects. Optical microscopy (OM) is the most frequently used non-destructive method to examine the surface of historical glasses; however, the 3D structural assessment of alteration layers requires applying the destructive modality of this technique to conduct a cross-sectional study. In this work, a different approach for structural and compositional characterization of alteration layers on model medieval-like glasses is presented, based on the combination of the laser spectroscopies of laser-induced breakdown spectroscopy (LIBS), laser-induced fluorescence (LIF) and FT-Raman, and the emerging, cutting edge technique of nonlinear optical microscopy (NLOM) in the modality of multiphoton excitation fluorescence (MPEF). The results obtained through this multi-analytical photonic approach were compared with those retrieved by examination of the surface and cross sections of the samples by OM and scanning electron microscopy–energy-dispersive X-ray spectroscopy (SEM–EDS). While the combination of LIBS, LIF and FT-Raman served to assess the composition of the various alteration layers, the use of MPEF microscopy allowed the non-destructive determination of the thicknesses of these layers, showing for both thickness and composition a good agreement with the OM and SEM–EDS results. Thus, the proposed approach, which avoids sample preparation, illustrates the capability of non-destructive, or micro-destructive in the case of LIBS, laser spectroscopies and microscopies for the in situ study of glass objects of historic or/and artistic value. Graphic Abstract
Flashed glasses are composed of a base glass and a thin colored layer and have been used since medieval times in stained glass windows. Their study can be challenging because of their complex composition and multilayer structure. In the present work, a set of optical and spectroscopic techniques have been used for the characterization of a representative set of flashed glasses commonly used in the manufacture of stained glass windows. The structural and chemical composition of the pieces were investigated by optical microscopy, field emission scanning electron microscopy-energy dispersive X-ray spectrometry (FESEM-EDS), UV-Vis-IR spectroscopy, laser-induced breakdown spectroscopy (LIBS), and laser-induced fluorescence (LIF). Optical microscopy and FESEM-EDS allowed the determination of the thicknesses of the colored layers, while LIBS, EDS, UV-Vis-IR, and LIF spectroscopies served for elemental, molecular, and chromophores characterization of the base glasses and colored layers. Results obtained using the micro-invasive LIBS technique were compared with those retrieved by the cross-sectional technique FESEM-EDS, which requires sample taking, and showed significant consistency and agreement. In addition, LIBS results revealed the presence of additional elements in the composition of flashed glasses that could not be detected by FESEM-EDS. The combination of UV-Vis-IR and LIF results allowed precise chemical identification of chromophores responsible for the flashed glass coloration.
The removal of aged varnish on artistic paintings is a delicate intervention and the use of UV laser for this purpose is of special relevance. In particular, the use of nanosecond-pulsed lasers operating at 213 nm has been noted to produce good results in mock-up samples, but it has not been tested in real artworks. In this paper, we report on the application of this procedure for the first time on a contemporary oil easel painting with naturally aged varnish. The obtained results were compared with those achieved using traditional solvents, specifically a mixture of ligroin:acetone. Additionally, hot water was used to remove surface dirt. The performance of the different cleaning procedures was assessed with a range of techniques, including low-power microscopy, UV lamp illumination, laser-induced fluorescence (LIF), and laser-induced breakdown spectroscopy (LIBS). Of the tested treatments, the best performance is obtained by nanosecond laser irradiation at 213 nm using an adequate laser fluence (typically 0.14 J/cm2) that allows controlled and efficient removal of the outermost aged varnish layer without affecting the underlying non-aged varnish and paint layers.
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