The role of relative humidity on crystallization of calcium carbonate from calcium acetoacetate precursor

Pondelak, Andreja; Rosi, Francesca; Maurich, Celeste; Miliani, Costanza; Škapin, Srečo D.; Škapin, Andrijana Sever

doi:10.1016/j.apsusc.2019.144768

Cited by 10 publications

(14 citation statements)

References 22 publications

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“…Calcite, vaterite, aragonite and ACC present similar FT-IR spectra, but with subtle differences in band positions, widths and relative intensities, which can be used to differentiate them 27,45,46 . In Fig.…”

Section: Resultsmentioning

confidence: 99%

“…2-], the shoulder peak at 850 cm -1 [out-of plane bending vibration (ν 2 ) of CO 3 27,45,46 . The absence of the peaks at 1709 cm -1 , 1,580 cm -1 and the CH stretching vibrational modes in the 3,000-2,800 cm -1 range (not shown) indicates that the consolidant precursor calcium acetoacetate is not present anymore in CFW.…”

Section: Resultsmentioning

confidence: 99%

“…Specifically, we have tested a newly developed calcium acetoacetate-based consolidant, as a precursor of CaCO 3 23 . Earlier studies have shown that different metastable calcium carbonate phases (i.e., first ACC followed by vaterite) can precede the formation of stable calcite in calcium-based consolidants (including those based on calcium acetoacetate) and that the formation of calcite is favored with increasing relative humidity (RH) [24][25][26][27] . Thus, for these specific systems, it is of major interest providing detailed information on the nature and distribution of the newly formed calcium carbonate crystalline phases and ACC directly in the stone porosity and on the environmental conditions at which they preferentially form.…”

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Synchrotron radiation Ca K-edge 2D-XANES spectroscopy for studying the stratigraphic distribution of calcium-based consolidants applied in limestones

Monico

Cartechini²,

Rosi³

et al. 2020

Sci Rep

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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 acetoacetatebased 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 semiquantitative 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. Stone consolidation is a major challenge for protection of buildings and stone artefacts from weathering and decay, which usually lead to decohesion of the structural elements of the material. Over the last decades, thanks to the progress in material science and nanotechnology, a wide range of novel materials has been developed, with the aim of re-establishing adhesion, cohesion and stability of the damaged stone as well as to improve efficacy and durability of the treatment 1,2. The effectiveness of a consolidation treatment depends on different aspects, including penetration depth, reaction kinetics and mechanism of formation of the final products, and physical-chemical properties of the consolidant phase in the stone matrix. In consideration of that, tailored analytical tools and methodologies have been developed to characterize newly synthesized consolidation products and to understand the chemistry behind their performances. Although

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Section: Resultsmentioning

confidence: 99%

Section: Resultsmentioning

confidence: 99%

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confidence: 99%

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Synchrotron radiation Ca K-edge 2D-XANES spectroscopy for studying the stratigraphic distribution of calcium-based consolidants applied in limestones

Monico

Cartechini²,

Rosi³

et al. 2020

Sci Rep

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“…The nanostructures of the aerogel samples were investigated with a Field Emission Scanning Electron Microscope (FESEM) [51,52]. Scanning electron microscopy operating at electron energies below 5 keV is usually termed Low Voltage Scanning Electron Microscopy (LVSEM) [53].…”

Section: Low Voltage Scanning Electron Microscopy (Lvsem)mentioning

confidence: 99%

False Morphology of Aerogels Caused by Gold Coating for SEM Imaging

et al. 2021

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The imaging of non-conducting materials by scanning electron microscopy (SEM) is most often performed after depositing few nanometers thick conductive layers on the samples. It is shown in this work, that even a 5 nm thick sputtered gold layer can dramatically alter the morphology and the surface structure of many different types of aerogels. Silica, polyimide, polyamide, calcium-alginate and cellulose aerogels were imaged in their pristine forms and after gold sputtering utilizing low voltage scanning electron microscopy (LVSEM) in order to reduce charging effects. The morphological features seen in the SEM images of the pristine samples are in excellent agreement with the structural parameters of the aerogels measured by nitrogen adsorption-desorption porosimetry. In contrast, the morphologies of the sputter coated samples are significantly distorted and feature nanostructured gold. These findings point out that extra care should be taken in order to ensure that gold sputtering does not cause morphological artifacts. Otherwise, the application of low voltage scanning electron microscopy even yields high resolution images of pristine non-conducting aerogels.

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“…22 In the presence of water, Ca(OAcAc) 2 transforms to CaCO 3 , acetone and carbon dioxide. [23][24][25] Under standard laboratory conditions (RT and 50% RH), this reaction is very slow, but the transformation is accelerated as temperature and relative humidity are increased. 23 The impregnation process of the mineralization procedure was therefore conducted at room temperature, then following treatment the temperature and relative humidity were increased to ensure that the desired reaction took place only once the impregnation solution had penetrated inside the wood.…”

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Improving the flame retardancy of wood using an eco-friendly mineralisation process

et al. 2021

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The role of relative humidity on crystallization of calcium carbonate from calcium acetoacetate precursor

Cited by 10 publications

References 22 publications

Synchrotron radiation Ca K-edge 2D-XANES spectroscopy for studying the stratigraphic distribution of calcium-based consolidants applied in limestones

Synchrotron radiation Ca K-edge 2D-XANES spectroscopy for studying the stratigraphic distribution of calcium-based consolidants applied in limestones

False Morphology of Aerogels Caused by Gold Coating for SEM Imaging

Improving the flame retardancy of wood using an eco-friendly mineralisation process

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