In Heritage Science, the evaluation of stone consolidation treatments by investigating the nature of in situ newly formed products and their penetration depth within the consolidated matrix is a grand challenge. A number of analytical methods have been proposed, but, currently, most of them are not able to supply a full overview of the spatial, structural and compositional information of the newly formed crystalline and amorphous phases with a submicrometric lateral resolution. Here, we examined, the capabilities of synchrotron radiation (SR)-based two-dimensional X-ray absorption near-edge structure (2D-XANES) spectroscopy at Ca K-edge for determining the structural and compositional properties of the compounds formed after the application of a calcium acetoacetate-based consolidant on a porous carbonatic stone (limestone) and for investigating their stratigraphic distribution at the submicrometric scale length. We evaluated advantages and drawbacks of three Ca K-edge 2D-XANES-based approaches: (i) transmission mode full-field-XANES (FF-XANES) imaging; (ii) micro-X-ray fluorescence (μ-XRF) mapping above the Ca K-edge combined with the acquisition of XRF mode μ-XANES spectra at a limited number of spots; (iii) full-spectral µ-XANES (FS µ-XANES) mapping in XRF mode and its variant called selectively induced X-ray emission spectroscopy (SIXES) mapping. Overall, Ca K-edge 2D-XANES spectroscopy provided accurate qualitative and semi-quantitative information on the newly formed calcium carbonates (i.e., amorphous calcium carbonate, vaterite and calcite) and their stratigraphic distribution at the submicrometric scale, thus opening a new scenario to study the carbonatation process of calcium-based consolidants in limestones.
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http://dx.doi.org/10.1038/s41598-020-71105-8 | DOI Listing |
Analyst
August 2024
Shanghai Institute of Applied Physics, Chinese Academy of Sciences, No. 2019 Jialuo Road, Shanghai, 201800, People's Republic of China.
Full-field transmission X-ray microscopy (TXM) in conjunction with X-ray absorption near edge structure (XANES) spectroscopy provides two-dimensional (2D) or three-dimensional (3D) morphological and chemical-specific information within samples at the tens of nanometer scale. This technique has a broad range of applications in materials sciences and battery research. Despite its extensive applicability, 2D XANES imaging is subject to the disadvantage of information overlap when the sample thickness is uneven.
View Article and Find Full Text PDFSci Rep
August 2020
Istituto di Scienze del Patrimonio Culturale (ISPC), CNR, Via Cardinale Guglielmo Sanfelice 8, 80134, Napoli, Italy.
J Synchrotron Radiat
March 2020
National Synchrotron Light Source II (NSLS-II), Upton, NY 11973, USA.
In the synchrotron X-ray community, X-ray absorption near-edge spectroscopy (XANES) is a widely used technique to probe the local coordination environment and the oxidation states of specific elements within a sample. Although this technique is usually applied to bulk samples, the advent of new synchrotron sources has enabled spatially resolved versions of this technique (2D XANES). This development has been extremely powerful for the study of heterogeneous systems, which is the case for nearly all real applications.
View Article and Find Full Text PDFNanoscale
June 2014
Department of Chemistry, The University of Western Ontario, 1151 Richmond Street, London, Ontario N6A 5B7, Canada.
Using 2D XANES-XEOL spectroscopy, it is found that the band gap emission of ZnO nanowire arrays is substantially enhanced i.e. that the intensity ratio between the band gap and defect emissions increases by more than an order of magnitude when the excitation energy is scanned across the O K-edge.
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