Development and trends in synchrotron studies of ancient and historical materials

Bertrand, Loïc; Cotte, Marine; Stampanoni, Marco; Thoury, Mathieu; Marone, Federica; Schöder, Sébastian

doi:10.1016/j.physrep.2012.03.003

Cited by 131 publications

(84 citation statements)

References 163 publications

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“…However, there are general reviews about the uses of synchrotron radiation applied to other fields like cultural heritage. [11,12] In particular, I found the second, very general, work [12] extremely enlightening. Furthermore, some techniques not treated here (because they have not been applied to building materials) are gathered and discussed there.…”

Section: A Very Brief Introduction To Synchrotron Radiation and Propementioning

confidence: 95%

Recent studies of cements and concretes by synchrotron radiation crystallographic and cognate methods

Aranda

2015

Crystallography Reviews

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The portfolio of available synchrotron radiation techniques is increasing notably for cements and pastes. Furthermore, sometimes the terminology is confusing and an overall picture highlighting similarities and differences of related techniques was lacking. Therefore, the main objective of this work is to review recent advances in synchrotron techniques providing a comprehensive overview. This work is not intended to gather all publications in cement chemistry but to give a unified picture through selected examples. Crystallographic techniques are used for structure determination, quantitative phase analyses and microstructure characterization. These studies are not only carried out in standard conditions but synchrotron techniques are especially suited to non-ambient conditions: high temperatures and pressures, hydration, etc., and combinations. Related crystallographic techniques, like Pair Distribution Function, are being used for the analysis of ill-crystalline phase(s). Furthermore, crystallographic tools are also employed in imaging techniques including scanning diffraction microscopy and tomography and coherent diffraction imaging. Other synchrotron techniques are also reviewed including X-rays absorption spectroscopy for local structure and speciation characterizations; small angle X-ray scattering for microstructure analysis and several imaging techniques for microstructure quantification: full-field soft and hard X-ray nano-tomographies; scanning infrared spectro-microscopy; scanning transmission and fluorescence X-ray tomographies. Finally, a personal outlook is provided.

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Section: A Very Brief Introduction To Synchrotron Radiation and Propementioning

confidence: 95%

Recent studies of cements and concretes by synchrotron radiation crystallographic and cognate methods

Aranda

2015

Crystallography Reviews

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“…30a. This fine structure, therefore, yields information about the distance to the surrounding atoms, as well as their number, and provides species identification of the neighbor atoms (Hayes and Boyce 1985;Bertrand et al 2012).…”

Section: Short-range Ordermentioning

confidence: 99%

The Structure of Semiconductors

Böer¹,

Pohl²

2014

Semiconductor Physics

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The bonding forces and atomic sizes determine the arrangement of the atoms in equilibrium in crystals. The crystal structure is determined by the tendency to fill a given space with the maximum number of atoms under the constraint of bonding forces and atomic radii. Crystal bonding and crystal structure are thus intimately related to each other and determine the intrinsic properties of semiconductors. Nonequilibrium states can be frozen-in and determine the structure of amorphous semiconductors. In an amorphous structure the short-range order is much like that in a crystal, while long-range periodicity does not exist. Quasicrystals are solids with an order between crystalline and amorphous. These quasiperiodic crystals have no three-dimensional translational periodicity, but exhibit long-range order in a diffraction experiment. A quasicrystalline pattern continuously fills all available space; unlike regular crystals space filling requires an aperiodic repetition of (at least) two different unit cells.Superlattices and low-dimensional structures like quantum wires and quantum dots, created by alternating thin depositions of different semiconductors, show material properties which can be engineered by designing size and chemical composition. This opens the feasibility for fabricating new and improved devices.

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“…n=64). In this way, FPA detectors provide in a short time (from tens of seconds to few minutes) information about identification and concentration of specific compounds and their distribution in the measured field of view, as each pixel gives an independent infrared spectrum corresponding to a different portion of the imaged area [3,4]. Spring et al [5] have illustrated the potential of micro-attenuated total reflection (ATR)-FTIRI and Joseph et al [6] of macro ATR-FTIRI for the characterisation of the material components of paint cross sections, allowing images to be obtained with spatial resolution of approximately 3-4 μm and 15 μm, respectively, gaining in both cases valuable information derived from the localisation of the compounds in the sample.…”

Section: Introductionmentioning

confidence: 99%

“…The FTIR images, plotted by integrating the CO 3 2− stretching band between 1550 and 1350 cm −1 , present the spatial distribution of CaCO 3 majorly in the ground layer ( Fig. 3g, h), whereas FTIR images obtained by integration of O-H stretching bands between 3730 and 3600 cm −1 , being characteristic of kaolinite, Al 2 Si 2 O 5 (OH) 4 , identify the kaolinitic nature of red ochre in the paint layer (Fig. 3i, k) [20].…”

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confidence: 99%

Improving FTIR imaging speciation of organic compound residues or their degradation products in wall painting samples, by introducing a new thin section preparation strategy based on cyclododecane pre-treatment

et al. 2015

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Fourier transform infrared (FTIR) imaging in transmission mode, employing a bidimensional focal plane array (FPA) detector, was applied for the detection and spatially resolved chemical characterisation of organic compounds or their degradation products within the stratigraphy of a critical group of fragments, originating from prehistoric and roman wall paintings, containing a very low concentration of subsisted organic matter or its alteration products. Past analyses using attenuated total reflection (ATR) or reflection FTIR on polished cross sections failed to provide any evidence of any organic material assignable as binding medium of the original painting. In order to improve the method's performance, in the present study, a new method of sample preparation in thin section was developed. The procedure is based on the use of cyclododecane C12H24 as embedding material and a subsequent double-side polishing of the specimen. Such procedure provides samples to be studied in FTIR transmission mode without losing the information on the spatial distribution of the detected materials in the paint stratigraphy. For comparison purposes, the same samples were also studied after opening their stratigraphy with a diamond anvil cell. Both preparation techniques offered high-quality chemical imaging of the decay products of an organic substance, giving clues to the painting technique. In addition, the thin sections resulting from the cyclododecane pre-treatment offered more layer-specific data, as the layer thickness and order remained unaffected, whereas the samples resulting from compression within the diamond cell were slightly deformed; however, since thinner and more homogenous, they provided higher spectral quality in terms of S/N ratio. In summary, the present study illustrates the appropriateness of FTIR imaging in transmission mode associated with a new thin section preparation strategy to detect and localise very low-concentrated organic matter subjected to deterioration processes, when the application of FTIR in reflection mode or FTIR-ATR fails to give any relevant information.

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Development and trends in synchrotron studies of ancient and historical materials

Cited by 131 publications

References 163 publications

Recent studies of cements and concretes by synchrotron radiation crystallographic and cognate methods

Recent studies of cements and concretes by synchrotron radiation crystallographic and cognate methods

The Structure of Semiconductors

Improving FTIR imaging speciation of organic compound residues or their degradation products in wall painting samples, by introducing a new thin section preparation strategy based on cyclododecane pre-treatment

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