Portable Apparatus for In Situ X-Ray Diffraction and Fluorescence Analyses of Artworks

2011 ◽  
Vol 17 (5) ◽  
pp. 667-673 ◽  
Author(s):  
Myriam Eveno ◽  
Brice Moignard ◽  
Jacques Castaing

AbstractA portable X-ray fluorescence/X-ray diffraction (XRF/XRD) system for artwork studies has been designed constructed and tested. It is based on Debye Scherrer XRD in reflection that takes advantage of many recent improvements in the handling of X-rays (polycapillary optics; advanced two-dimensional detection). The apparatus is based on a copper anode air cooled X-ray source, and the XRD analysis is performed on a 5–20 μm thick layer from the object surface. Energy dispersive XRF elemental analysis can be performed at the same point as XRD, giving elemental compositions that support the interpretation of XRD diagrams. XRF and XRD analyses were tested to explore the quality and the limits of the analytical technique. The XRD diagrams are comparable in quality with diagrams obtained with conventional laboratory equipment. The mineral identification of materials in artwork is routinely performed with the portable XRF-XRD system. Examples are given for ceramic glazes containing crystals and for paintings where the determination of pigments is still a challenge for nondestructive analysis. For instance, lead compounds that provide a variety of color pigments can be easily identified as well as a pigment such as lapis lazuli that is difficult to identify by XRF alone. More than 70 works of art have been studied in situ in museums, monuments, etc. In addition to ceramics and paintings, these works include bronzes, manuscripts, etc., which permit improvement in the comprehension of ancient artistic techniques.

Author(s):  
Nicholas Armstrong ◽  
Peter A. Lynch ◽  
Sitarama R. Kada ◽  
Pavel Cizek ◽  
Justin A. Kimpton ◽  
...  

Abstract Linking the accumulation of microstructural damage prior to crack initiation to the lifing of aero-engines components would help to better predict the time that a component spends in this crack initiation stage. We present the results and analysis of in-situ high-resolution X-ray diffraction (XRD) experiments of a Ti-6Al-4V specimen that experienced tensile loading using medium energy synchrotron X-rays (≤ 21 keV) carried out at the Australian Synchrotron. The XRD analysis characterised XRD line-broadening due to the build-up of dislocations and the formation of crystallites in α- and β-Ti-6Al-4V specimens. Using Bayesian XRD analysis methods, the density, spatial arrangement of dislocations, and crystallite size information for α- and β-phases of the Ti-6Al-4V was extracted from the XRD line-profiles, as a function of applied load. The XRD analysis was then compared and validated with transmission electron microscopy (TEM) analysis of the specimen before and after the loading. Comparison of the TEM and XRD analysis reveals broad agreement in terms of the microstructural damage of Ti-6Al-4V specimens.


2007 ◽  
Vol 130 ◽  
pp. 7-14 ◽  
Author(s):  
Andrew N. Fitch

The highly-collimated, intense X-rays produced by a synchrotron radiation source can be harnessed to build high-resolution powder diffraction instruments with a wide variety of applications. The general advantages of using synchrotron radiation for powder diffraction are discussed and illustrated with reference to the structural characterisation of crystalline materials, atomic PDF analysis, in-situ and high-throughput studies where the structure is evolving between successive scans, and the measurement of residual strain in engineering components.


2000 ◽  
Vol 07 (04) ◽  
pp. 437-446 ◽  
Author(s):  
G. RENAUD

The application of X-rays to the structural characterization of surfaces and interfaces, in situ and in UHV, is discussed on selected examples. Grazing incidence X-ray diffraction is not only a very powerful technique for quantitatively investigating the atomic structure of surfaces and interfaces, but is also very useful for providing information on the interfacial registry for coherent interfaces or on the strain deformation, island and grain sizes for incoherent epilayers.


2011 ◽  
Vol 26 (2) ◽  
pp. 134-137 ◽  
Author(s):  
K. Matsui ◽  
A. Ogawa ◽  
J. Kikuma ◽  
M. Tsunashima ◽  
T. Ishikawa ◽  
...  

Hydrothermal formation reaction of tobermorite in the autoclaved aerated concrete (AAC) process has been investigated by in situ X-ray diffraction. High-energy X-rays from a synchrotron radiation source in combination with a newly developed autoclave cell and a photon-counting pixel array detector were used. XRD measurements were conducted in a temperature range 100–190°C throughout 12 h of reaction time with a time interval of 4.25 min under a saturated steam pressure. To clarify the tobermorite formation mechanism in the AAC process, the effect of Al addition on the tobermorite formation reaction was studied. As intermediate phases, non-crystalline calcium silicate hydrate (C-S-H), hydroxylellestadite (HE), and katoite (KA) were clearly observed. Consequently, it was confirmed that there were two reaction pathways via C-S-H and KA in the tobermorite formation reaction of Al containing system. In addition, detailed information on the structural changes during the hydrothermal reaction was obtained.


2015 ◽  
Vol 88 (1) ◽  
pp. 138-146 ◽  
Author(s):  
Rouhollah Bagheri ◽  
Reza Darvishi

ABSTRACT In this study, polyurethane (PU)/organomodified montmorillonite (cloisite®30B) is synthesized via in situ polymerization by reaction of an ether-based prepolymer with the isocyanate end groups and adiamine chain extender (4, 4-methylene-bis(2-chloroaniline)) in the presence of different amounts of nanoparticles dispersed in the prepolymer matrix by an ultrasonic mixer for 1 h. The synthesized polymers are cast on a pretreated carbon steel sheet and cured at 120 °C in an oven. The PU and its composites have been characterized by using Fourier transform infrared spectroscopy, X-ray diffraction (XRD), and mechanical testing. The XRD analysis of the cured samples containing 1 to 3 wt% cloisite30B showed intercalation segments in the silicate layers and exfoliation for 0.5 wt% nanoparticles. The highest mechanical properties were obtained using the cured exfoliated silicate layer sample. A twofold increase in the ultimate tensile strength and a 2.3 times increase in the adhesion strength were found for 0.5 wt% organoclay/PU as compared with that of pure PU. In addition, the exfoliated structure sample exhibited a 16% reduction in abrasion compared with that of pure PU.


1999 ◽  
Vol 13 (09n10) ◽  
pp. 991-996
Author(s):  
M. Salvato ◽  
C. Attanasio ◽  
G. Carbone ◽  
T. Di Luccio ◽  
S. L. Prischepa ◽  
...  

High temperature superconducting multilayers have been obtained depositing Bi2Sr2CuO6+δ(2201) and ACuO2 layers, where A is Ca or Sr, by Molecular Beam Epitaxy (MBE) on MgO and SrTiO3 substrates. The samples, formed by a sequence of 2201/ACuO2 bilayers, have different thickness of ACuO2 layers while the thickness of the 2201 layers is kept constant. The surface structure of each layer has been monitored by in situ Reflection High Energy Electron Diffraction (RHEED) analysis which has confirmed a 2D nucleation growth. X-ray diffraction (XRD) analysis has been used to confirm that the layered structure has been obtained. Moreover, one-dimensional X-ray kinematic diffraction model has been developed to interpret the experimental data and to estimate the period of the multilayers. Resistive measurements have shown that the electrical properties of the samples strongly depend on the thickness of the ACuO2 layers.


1998 ◽  
Vol 69 (2) ◽  
pp. 512-516 ◽  
Author(s):  
G. Scherb ◽  
A. Kazimirov ◽  
J. Zegenhagen

2006 ◽  
Vol 13 (02n03) ◽  
pp. 155-166 ◽  
Author(s):  
WOLFGANG BRAUN ◽  
KLAUS H. PLOOG

X-rays are ideal to study the structure of crystals due to their weak interaction with matter and in most cases allow a quantitative analysis using kinematical theory. To study the incorporation of atoms during crystal growth and to analyze the kinetics on the crystal surface high primary beam intensities available at synchrotrons are required. Our studies of the molecular beam epitaxy growth of III–V semiconductors reveal that, despite their similarity in crystal structure, the surface kinetics of GaAs (001), InAs (001) and GaSb (001) differ strongly. GaAs shows an unexpectedly large coarsening exponent outside the predicted range of Ostwald ripening models during recovery. GaSb exhibits dramatically different surface morphology variations during growth and recovery. Overgrowth of GaAs by epitaxial MnAs demonstrates the ability of X-ray diffraction to follow an interface as it is buried during heteroepitaxy, which is not possible by reflection high-energy electron diffraction.


2006 ◽  
Vol 519-521 ◽  
pp. 1569-1578
Author(s):  
Dorte Juul Jensen

By 3 dimensional X-ray diffraction (3DXRD) using high energy X-rays from synchrotron sources it is possible to study in-situ the nucleation and growth during recrystallization. In this paper it is described and discussed how 3DXRD can supplement EBSP measurements of nucleation and growth. Three types of studies are considered: i) orientation relationships between nuclei and parent deformed matrix, ii) recrystallization kinetics of individual bulk grains and iii) filming of growing grains in deformed single crystals.


No X-ray diffraction photographs have yet been obtained of muscle in the very act of contracting or relaxing, but much work has been carried out in the approaches to this goal. I reviewed the situation in 1945 in my Croonian Lecture (Astbury 1947 a ), and the present contribution may serve partly to recall some of the main conclusions already arrived at then, but chiefly to develop them in relation to more recent discoveries. In all the kinds of muscles that have so far been examined by X-rays the dominating feature has been found to be the fibrous protein myosin lying along the direction of the myofibrils; further structural components have been revealed according to the type of muscle, it is true, but myosin at least seems to be essential, and there are very strong reasons, not only from X-rays but from much other evidence besides, for believing that it is indeed the mainspring of the contractile apparatus proper. Many X-ray and accessory studies have been carried out on it both in situ and after extraction, and it is a principal inference from such investiga­tions that, whatever the detailed steps by which contraction and recovery are contrived in muscle itself, myosin has at any rate properties peculiarly fitted for these purposes. The myosin molecule or complex is inherently elastic; it can be caused to change its internal configuration and thereby alter its length over a large range.


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