共查询到20条相似文献,搜索用时 31 毫秒
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2.
Loïc Bertrand Marine Cotte Marco Stampanoni Mathieu Thoury Federica Marone Sebastian Schöder 《Physics Reports》2012
Synchrotron photon-based methods are increasingly being used for the physico-chemical study of ancient and historical materials (archaeology, palaeontology, conservation sciences, palaeo-environments). In particular, parameters such as the high photon flux, the small source size and the low divergence attained at the synchrotron make it a very efficient source for a range of advanced spectroscopy and imaging techniques, adapted to the heterogeneity and great complexity of the materials under study. The continuous tunability of the source — its very extended energy distribution over wide energy domains (meV to keV) with a high intensity — is an essential parameter for techniques based on a very fine tuning of the probing energy to reach high chemical sensitivity such as XANES, EXAFS, STXM, UV/VIS spectrometry, etc. The small source size attained (a few micrometres) at least in the vertical plane leads to spatial coherence of the photon beams, giving rise in turn to a series of imaging methods already crucial to the field. This review of the existing literature shows that microfocused hard X-ray spectroscopy (absorption, fluorescence, diffraction), full-field X-ray tomography and infrared spectroscopy are the leading synchrotron techniques in the field, and presents illustrative examples of the study of ancient and historical materials for the various methods. Fast developing analytical modalities in scanning spectroscopy (STXM, macro-XRF scanning) and novel analytical strategies regarding optics, detectors and other instrumental developments are expected to provide major contributions in the years to come. Other energy domains are increasingly being used or considered such as far-infrared and ultraviolet/visible for spectroscopy and imaging. We discuss the main instrumental developments and perspectives, and their impact for the science being made on ancient materials using synchrotron techniques. 相似文献
3.
B. Kanngießer W. Malzer I. Mantouvalou D. Sokaras A. G. Karydas 《Applied Physics A: Materials Science & Processing》2012,106(2):325-338
Quantitative X-ray fluorescence (XRF) and particle induced X-ray emission (PIXE) techniques have been developed mostly for
the elemental analysis of homogeneous bulk or very simple layered materials. Further on, the microprobe version of both techniques
is applied for 2D elemental mapping of surface heterogeneities. At typical XRF/PIXE fixed geometries and exciting energies
(15–25 keV and 2–3 MeV, respectively), the analytical signal (characteristic X-ray radiation) emanates from a variable but
rather extended depth within the analyzed material, according to the exciting probe energy, set-up geometry, specimen matrix
composition and analyte. Consequently, the in-depth resolution offered by XRF and PIXE techniques is rather limited for the
characterization of materials with micrometer-scale stratigraphy or 3D heterogeneous structures. This difficulty has been
over-passed to some extent in the case of an X-ray or charged particle microprobe by creating the so-called confocal geometry.
The field of view of the X-ray spectrometer is spatially restricted by a polycapillary X-ray lens within a sensitive microvolume
formed by the two inter-sectioned focal regions. The precise scanning of the analyzed specimen through the confocal microvolume
results in depth-sensitive measurements, whereas the additional 2D scanning microprobe possibilities render to element-specific
3D spatial resolution (3D micro-XRF and 3D micro-PIXE). These developments have contributed since 2003 to a variety of fields
of applications in environmental, material and life sciences. In contrast to other elemental imaging methods, no size restriction
of the objects investigated and the non-destructive character of analysis have been found indispensable for cultural heritage
(CH) related applications. The review presents a summary of the experimental set-up developments at synchrotron radiation
beamlines, particle accelerators and desktop spectrometers that have driven methodological developments and applications of
confocal X-ray microscopy including depth profiling speciation studies by means of confocal X-ray absorption near edge structure
(XANES) spectroscopy. The solid mathematical formulation developed for the quantitative in-depth elemental analysis of stratified
materials is exemplified and depth profile reconstruction techniques are discussed. Selected CH applications related to the
characterization of painted layers from paintings and decorated artifacts (enamels, glasses and ceramics), but also from the
study of corrosion and patina layers in glass and metals, respectively, are presented. The analytical capabilities, limitations
and future perspectives of the two variants of the confocal micro X-ray spectroscopy, 3D micro-XRF and 3D micro-PIXE, with
respect to CH applications are critically assessed and discussed. 相似文献
4.
Monia Vadrucci Anna Mazzinghi Beatrice Sorrentino Stella Falzone Claudia Gioia Patrizia Gioia Ersilia M. Loreti Massimo Chiari 《X射线光谱测定》2020,49(6):668-678
Scientific investigation is very important in studies addressing issues of archaeological and historical objects. Ion beam analysis (IBA) and macro X-ray fluorescence (MA-XRF) spectroscopy are remarkable tools to obtain information about elemental composition and imaging of historical artefacts with a non-invasive character. These investigation techniques were employed in the framework of a project aimed at supporting the characterization of materials and techniques related with the Roman wall painting. The archaeological excavations at Villa della Piscina in Rome have revealed a luxury building with a large pool (about 50 m long) and thermal baths and numerous fragments of plaster, coming from intentional demolitions referable to two distinct architectural contexts of the Villa during the imperial age, have been found. This work deals with studying the interesting wall pictorial apparatus of great cultural value of the heritage inherited from the Roman age in the area of the ancient city of Rome. The colour palette of the pigments investigated, in particular, by MA-XRF and particle-induced X-ray emission (PIXE) and has revealed Fe, Cu, Pb, Si and Hg as main elements. Traces of other constituents uncover the choice of the different colours chosen by the artists who had embellished the rooms of the Villa. 相似文献
5.
S. Reguer P. Dillmann F. Mirambet J. Susini P. Lagarde 《Applied Physics A: Materials Science & Processing》2006,83(2):189-193
Synchrotron-based micro-X-ray absorption spectroscopy is used in the present study to obtain chemical information at the microscopic
scale such as coordination and oxidation state of Fe atoms in phases constituting corrosion products within archaeological
iron artefacts buried in soil. This technique is required in order to answer questions about the iron corrosion process related
to the presence of chloride, particularly for restoration and conservation of metallic artefacts of the cultural heritage.
The samples available for X-ray microprobe analyses are cross sections from corroded iron archaeological objects. Previously,
complementary techniques have been used such as μXRD and μRaman. This specific study applies micro-X-ray absorption spectroscopy
to determine the spatial variation of the predominant Fe oxidation state and to identify the corresponding crystallographic
phase. The analyses performed at Fe and Cl K-edges (μXANES) reveal the correlation between the valence distribution in the
corrosion products and the evolution of the chloride concentration. In addition to the presence of the well-known iron oxyhydroxide
β-FeOOH: akaganeite, we highlight the presence of another important phase, the β-Fe2(OH)3Clhydroxychloride. These important findings help to gain new insights concerning the influence of such phases in the iron
corrosion mechanism within their precise characterization.
PACS 61.10.Ht; 61.10.-i; 68.49.Uv 相似文献
6.
Ceramic tiles used to manufacture artistic panels during the XVI to the XVIII centuries were decorated with high-lead soda-lime
glazes, incorporating a diversity of chromophore cations, as ascertained by SRXRF (synchrotron radiation X-ray fluorescence).
Previous X-ray absorption spectroscopy (XAS) studies have shown that sodium and lead are hosted by the glassy matrix in those
glazes. However, the possible role of calcium as a modifier of the tetrahedral silica network is not fully clarified, despite
being recognized that calcium cations alter some fundamental properties of glazes, namely transparency. An X-ray absorption
fine structure (XAFS) study of glazes with varied colorings was therefore undertaken at Ca K- and L-edges. Well crystallized
oxide minerals were used to model distinct coordination environments by oxygen atoms – close to octahedral geometry in calcite
and dodecahedral in gypsum – while fluorite was chosen to mimic ideal cubic coordination. A first XAS approach suggested a
minor variation in the energy separation between L2–L3 absorption edges when comparing blue and yellow glazes, irrespective of the period of manufacture. A further study on the
X-ray absorption near-edge structure (XANES) carried out at the K-edge corroborated this difference and, along with the theoretical
spectra modeling performed with the FEFF code, allowed interpreting of the Ca 1s absorption spectra of glazes as arising from
a non-regular high-coordination environment within the silica matrix.
PACS 61.43.Fs; 41.60.Ap; 61.10.Ht 相似文献
7.
M.O. Figueiredo T.P. Silva J.P. Veiga 《Applied Physics A: Materials Science & Processing》2006,83(2):209-211
Aged lead-rich, tin-opacified glazes from polychrome tiles manufactured in the 16th–18th century were studied to ascertain
the structural role of lead. Glaze fragments with white, blue, yellow, brown and green colouring were analysed using non-destructive
X-ray techniques, both laboratorial – X-ray diffraction to identify crystalline components – and synchrotron-based. Elemental
analyses by synchrotron radiation X-ray fluorescence were performed at the former LURE photon microprobe (line D15A at DCI,
in Orsay). The instrumental set-up of beamline BM29 at the ESRF, in Grenoble, was applied to collect X-ray absorption spectra
at the Pb L3-edge. Natural minerals and synthetics with known crystal structure were used as model oxy-compounds to configure different
formal valences and coordinations of lead ions by oxygen anions, and to interpret the effects upon details of X-ray absorption
near-edge spectroscopy (XANES) spectra. Experimental evidence supports the general conclusion that lead is hosted by the glassy
matrix, irrespective of the glaze colour. Furthermore, it was concluded that lead ions assume coordinations higher than usual
for silica glasses, acting as network modifiers in the silica-lime-alkali glasses of ancient tile glazes.
PACS 61.43.Fs; 41.60.Ap; 61.10.Ht 相似文献
8.
Minerals, as raw structural materials or pigments, play a fundamental role in archaeometry, for the understanding of nature, structure and status of an artefact or object of interest for cultural heritage. A detailed knowledge of the mineral phases is crucial to solve archaeological problems: Raman spectroscopy is a powerful investigation technique and has been applied extensively in the last 30 years on mineral identification and on pigment degradation. Here we report an updated review, covering the last decade, of the applications of Raman techniques to issues in which raw minerals, including mineral pigments, are involved. Particular attention is devoted to cases where the Raman analysis of minerals is deeper than a simple identification of the phases present in an archaeological or artistic object. Copyright © 2016 John Wiley & Sons, Ltd. 相似文献
9.
Idham Hafizh Giovanni Bellotti Marco Carminati Gianlorenzo Utica Matteo Gugiatti Antonella Balerna Vinicio Tullio Giacomo Borghi Antonio Picciotto Francesco Ficorella Nicola Zorzi Andrea Capsoni Simone Coelli Luca Bombelli Carlo Fiorini 《X射线光谱测定》2019,48(5):382-386
ARDESIA, a four-channel X-ray spectrometer based on silicon drift detectors (SDDs), is presented. It has been developed for synchrotron applications targeting especially X-ray fluorescence (XRF) and X-ray absorption spectroscopy (XAS) with good energy resolution at high count rates (a few Mcps per second). The main target applications are XRF and XAFS techniques. The system features a 2 × 2 monolithic array of 5-mm-pitch SDDs cooled with a double Peltier scheme and coupled to a four-channel CUBE charge preamplifier. Different digital pulse processors allowing operation in Mcps per second count rates are employed. The results of preliminary characterization measurements performed at both the LNF DAΦNE-Light DXR1 beamline and the ESRF LISA BM-08 are reported, in particular, XRF measurements on low atomic number elements (down to the Carbon K-line, 270 eV) and extended X-ray absorption fine structure of trace materials in pyrite. 相似文献
10.
G. Van der Snickt W. De Nolf B. Vekemans K. Janssens 《Applied Physics A: Materials Science & Processing》2008,92(1):59-68
For the non-destructive identification of pigments and colorants in works of art, in archaeological and in forensic materials,
a wide range of analytical techniques can be used. Bearing in mind that every method holds particular limitations, two complementary
spectroscopic techniques, namely confocal μ-Raman spectroscopy (μ-RS) and μ-X-ray fluorescence spectroscopy (μ-XRF), were
joined in one instrument. The combined μ-XRF and μ-RS device, called PRAXIS unites both complementary techniques in one mobile
setup, which allows μ- and in situ analysis. μ-XRF allows one to collect elemental and spatially-resolved information in a
non-destructive way on major and minor constituents of a variety of materials. However, the main disadvantages of μ-XRF are
the penetration depth of the X-rays and the fact that only elements and not specific molecular combinations of elements can
be detected. As a result μ-XRF is often not specific enough to identify the pigments within complex mixtures. Confocal Raman
microscopy (μ-RS) can offer a surplus as molecular information can be obtained from single pigment grains. However, in some
cases the presence of a strong fluorescence background limits the applicability. In this paper, the concrete analytical possibilities
of the combined PRAXIS device are evaluated by comparing the results on an illuminated sheet of parchment with the analytical
information supplied by synchrotron radiation μ-X-ray diffraction (SR μ-XRD), a highly specific technique.
PACS 33.20.Fb; 61.05.cp; 33.20.Rm; 07.85.Qe; 91.65.An 相似文献
11.
L. Bertrand D. Vantelon E. Pantos 《Applied Physics A: Materials Science & Processing》2006,83(2):225-228
The information that can be retrieved from the study of ancient materials and studies on their conservation rely strongly
on the development and application of new techniques of physical analysis. This is particularly important at a time when global
changes affecting our environment and way of life impose new stresses putting heritage preservation at risk. For this purpose,
synchrotron techniques are particularly suited to the non- (or micro-) destructive characterisation of such heterogeneous
materials, and a steep increase in the number of publications has been noticed recently from cultural heritage works using
synchrotron radiation.
In 2004, an interface dedicated to archaeology and cultural heritage was launched at the SOLEIL synchrotron to allow researchers
from the international scientific community to be granted specific expertise. This interface aims at easing the access of
researchers to the synchrotron, facilitating contacts, providing technical support and informing the community. The very first
applications of SOLEIL beamlines in the heritage field are illustrated through works recently carried out at the first beamline
of SOLEIL, LUCIA, currently located at the Swiss Light Source (SLS). The setup of the beamline is succinctly described.
PACS 07.85.Qe; 87.59.-e 相似文献
12.
J. Arthur 《Il Nuovo Cimento D》1996,18(2-3):213-220
Summary The use of synchrotron radiation to excite low-lying nuclear resonances is a rapidly developing field showing great promise
for hyperfine spectroscopy, phonon spectroscopy and kinetic studies, crystallography, and fundamental physics experiments.
Recent technical advances in synchrotron sources, optics, and fast detectors have drastically increased signal rates and expanded
the range of samples that can be studied. A typical experiment today uses a high-brightness synchrotron source having X-ray
pulses well-separated in time, a meV-bandpass monochromator using perfect crystals of silicon or germanium, a sample containing
resonant nuclei, and an avalanche photodiode timing detector. Both coherent and incoherent scattering can be observed; the
coherent scattering is used for hyperfine spectroscopy and studies of diffraction interference phenomena, and the incoherent-scattering
signal promises to be very useful for phonon spectroscopy and other studies of excitations in condensed systems. At this point
seven nuclear isotopes have been used to resonantly scatter synchrotron radiation, but the number is rapidly increasing.
Paper presented at the ICAME-95, Rimini 10–16 September 1995. 相似文献
13.
P. K. Khanna K. Srinivasa Rao K. R. Patil V. N. Singh B. R. Mehta 《Journal of nanoparticle research》2010,12(1):101-109
Surface-capped CdSe and CdTe nano-crystals (NCs) have been synthesized using cadmium acetate, oleic acid and respective tri-octylphosphine
chalcogenide (TOPE; E = Se/Te) in diphenyl ether (DPE). Well-dispersed CdSe particles showed two absorption bands at the region
of 431–34 and 458–60 nm in optical absorption study. A band-edge emission resulted at 515 nm with an excitation energy of
400 nm, in its photoluminescence (PL) spectrum. Similarly, UV–visible absorption study of CdTe revealed an absorption band
at <700 nm. The broadened X-ray diffraction (XRD) pattern showed that at higher reaction temperature cubic CdSe but hexagonal
CdTe can be obtained with crystallite size of <10 nm. Scanning electron microscopy (SEM) and transmission electron microscopy
(TEM) revealed that agglomerated particles are of spherical nature. The inter-planar spacing in CdTe was measured to be 0.406 nm,
a characteristic of (100) lattice plane in hexagonal CdTe. X-ray photoelectron spectroscopy (XPS) showed that CdSe NCs have
better air stability stable than CdTe. Presence of organic moiety around the semiconductor particles was confirmed by infra-red
(IR) spectroscopy. 相似文献
14.
Fabrizio Bardelli Germana Barone Vincenza Crupi Francesca Longo Giacomo Maisano Domenico Majolino Paolo Mazzoleni Valentina Venuti 《Journal of synchrotron radiation》2012,19(5):782-788
The present work reports a detailed investigation on the speciation of iron in the pigments of decorated pottery fragments of cultural heritage relevance. The fragments come from the Gioiosa Guardia archaeological site in the area of the `Strait of Messina' (Sicily, Southern Italy), and date back to VI–V century BC. The purpose of this study is to characterize the main pigmenting agents responsible for the dark‐red coloration of the specimens using non‐destructive analytical techniques such as synchrotron radiation X‐ray absorption spectroscopy (SR‐XAS), a well established technique for cultural heritage and environmental subjects. Absorption spectra were collected at the Fe K‐edge on the Italian beamline for absorption and diffraction (BM8‐GILDA) at the European Synchrotron Radiation Facility in Grenoble (France). In order to determine the speciation of Fe in the samples, principal component analysis and least‐squares fitting procedures were applied to the near‐edge part of the absorption spectra (XANES). Details on the local structure around the Fe sites were obtained by analyzing the extended part of the spectra (EXAFS). Furthermore, an accurate determination of the average Fe oxidation state was carried out through analysis of the pre‐edge peaks of the absorption spectra. Samples resulted composed of an admixture of Fe2O3 (hematite or maghemite) and magnetite (Fe3O4), occurring in different relative abundance in the dark‐ and light‐colored areas of the specimens. The results obtained are complementary to information previously obtained by means of instrumental neutron activation analysis, Fourier transform infrared absorbance and time‐of‐flight neutron diffraction. 相似文献
15.
I. S. Lyubutin A. G. Gavriliuk 《Bulletin of the Russian Academy of Sciences: Physics》2007,71(11):1594-1598
The latest results of experimental study of the effect of high pressure on the magnetic and crystal structures, electronic
and spin states, and transport properties of some 3d-metal oxides with different crystal structures are reported. Along with the X-ray diffraction, optical absorption spectroscopy,
and Raman spectroscopy, direct resistivity measurements have been performed and several techniques based on synchrotron radiation
were used to carry out high-pressure experiments in diamond anvil cells.
Original Russian Text 7sC I.S. Lyubutin, A.G. Gavriliuk, 2007, published in Izvestiya Rossiiskoi Akademii Nauk. Seriya Fizicheskaya,
2007, Vol. 71, No. 11, pp. 1635–1639. 相似文献
16.
C. T. Chantler 《The European physical journal. Special topics》2009,169(1):147-153
Over recent synchrotron experiments and publications we have devel- oped methods for measuring the absorption coefficient
in the XAFS (X-ray Absorption Fine Structure) region and far from an edge in neutral atoms, simple compounds and organometallics
which can reach accuracies of below 0.02%. This is 50–500 times more accurate than earlier methods, and 50–250 times more
accurate than claimed uncertainties in theoretical computations for these systems. The data and methodology is useful for
a wide range of applications, including dominant synchrotron and laboratory techniques relating to fine structure, near-edge
analysis and standard crystallography. The experiments are sensitive to many theoretical and computational issues, including
correlation and convergence of individual electronic and atomic orbitals and wavefunctions. 相似文献
17.
M.O. Figueiredo T.P. Silva J.P. Veiga 《Applied Physics A: Materials Science & Processing》2008,92(1):151-154
A review is presented on constructive techniques plus materials and the processes involved in degradation phenomena observed
in two historical monuments: the Zambujeiro dolmen (Portugal) and the Roman Aqueduct of Carthage (Tunisia).
Dolmens are particularly impressive megalithic constructions for the dimensions of granite blocks. At Zambujeiro, the upright
stones have undergone a catastrophic evolution after the archaeological exploitation due to accelerated weathering through
a process apparently distinct from natural granite decay in nearby outcrops. The biological attack of granite minerals by
lichen exudates has emphasized the hazardous character of bromine and more has been learnt about construction techniques,
namely, the insertion in the mound of an impermeable clay stratum that hinders water penetration into the dolmen chamber.
The characterization of original Roman ashlar blocks, including masonry and the diagnosis of Byzantine and medieval reconstruction
testimonies in the Aqueduct of Carthage were the object of a detailed study by X-ray diffraction and synchrotron radiation
X-ray fluorescence. Traditional constructive techniques and local construction materials were studied and successive historical,
modern and recent rehabilitations were reappraised.
PACS 83.80.Nb; 64.70.Kb; 78.70.En; 41.60.Ap 相似文献
18.
S. Padovani F. D'Acapito E. Cattaruzza A. De Lorenzi F. Gonella G. Mattei C. Maurizio P. Mazzoldi M. Montagna S. Ronchin C. Tosello M. Ferrari 《The European Physical Journal B - Condensed Matter and Complex Systems》2002,25(1):11-17
Composite silica films containing metal nanoclusters were prepared by the rf- sputtering technique, in which SiO2 was co-deposited with gold+copper, gold+silver, or copper+silver. The formation of either pure or alloy clusters was studied
by extended X-ray absorption fine structure spectroscopy and transmission electron microscopy. For all systems, the presence
of alloy aggregates was evidenced. Moreover, small amounts of pure metal aggregates as well as dispersed or oxidized dopants
were observed.
61.46.+w Nanoscale materials: clusters, nanoparticles, nanotubes, and nanocrystals – 61.10.Ht X-ray absorption spectroscopy:
EXAFS, NEXAFS, XANES, etc. – 81.05.Pj Glass-based composites, vitroceramics
Received 29 June 2001 相似文献
19.
Rima Paul Arnab Maity Arindam Mitra Pathik Kumbhakar Apurba Krishna Mitra 《Journal of nanoparticle research》2011,13(11):5749-5757
Ag nanoparticles of average size 20 nm have been deposited on SWCNT surfaces following a very lucid wet chemical process.
The SWCNT/Ag nanohybrid material has been characterized using scanning electron microscopy (SEM), energy dispersive X-ray
analysis (EDAX), X-ray diffraction (XRD) analysis and Raman spectroscopy. Both optical and electrical properties of the hybrid
have been studied. The hybrid material has been synthesized at 60 °C and treated to higher temperatures. About three-fold
increase in photoluminescence (PL) emission intensity has been achieved when the hybrid sample has been treated to 500 °C.
DC conductivity at varying temperatures from 77–473 K has been studied. The conductivity of Ag-decorated SWCNTs increased
up to 1.76 times of that of pristine SWCNT at a low temperature of 180 K. This hybrid material can find wide application as
conducting filler in polymer composite which other filler materials seldom possess. 相似文献
20.
D. Barilaro V. Crupi S. Interdonato D. Majolino V. Venuti G. Barone M.F. La Russa F. Bardelli 《Applied Physics A: Materials Science & Processing》2008,92(1):91-96
Renaissance blue decorated pottery fragments from the archaeological site of Caltagirone (Sicily, Italy) were analysed by
scanning electron microscopy – energy dispersive X-ray spectrometry (SEM/EDS). The samples were dated back to 16th century
AD on the basis of archaeological observations. The micro-chemical analyses were performed on the ceramic body and the surface
decorated layer of the samples. Particularly, the investigation was addressed the characterization of the coating blue decorations.
The obtained results allowed us to clearly identify smalt as pigment. Also the presence of arsenic (As) was revealed and the
Co/As ratio values were calculated and related to the different process used for the pigment preparation. Further spectroscopic
analyses, performed through X-ray absorbance spectroscopy (XAS), carried out at the Co K-edge, confirmed the micro-analytical
results and permitted us to identify the oxidation form and the local environment of cobalt atoms.
PACS 81.05.Mh; 82.80.-d; 68.37.Hk 相似文献