Towards three-dimensional quantitative reconstruction of cement microstructure by X-ray diffraction microtomography

2011 ◽  
Vol 44 (2) ◽  
pp. 272-280 ◽  
Author(s):  
Luca Valentini ◽  
Maria Chiara Dalconi ◽  
Matteo Parisatto ◽  
Giuseppe Cruciani ◽  
Gilberto Artioli

Quantitative characterization of the microstructure of cement-based materials is of fundamental importance for assessing the performance and durability of the final products. However, accessing the three-dimensional microstructural information of hydrating cement pastes without introducing any perturbation is not trivial. Recently, a novel non-invasive method based on X-ray diffraction computed microtomography (XRD-CT) has been applied to cement-based materials, with the aim of describing the three-dimensional spatial distribution of selected phases during the hydration of the cement paste. This paper illustrates a method based on XRD-CT, combined with Rietveld-based quantitative phase analysis and image processing, which provides quantitative information relative to the distribution of the various phases present in the studied samples. In particular, it is shown how this method allows the estimation of the local volume fraction of the phase ettringite within a hydrating cement paste, and construction of a three-dimensional distribution map. Application of this method to the various constituents of a cementitious material, or, more generally, of a composite polycrystalline material, may provide a non-invasive tool for three-dimensional microstructural quantitative characterization.

1987 ◽  
Vol 2 (2) ◽  
pp. 96-98 ◽  
Author(s):  
Jacques Renault

AbstractXRF and XRD measurements made on a single pressed powder briquet can be combined to give more quantitative information than either technique employed alone. Speed of analysis and simplification of sample preparation are also enhanced. The algorithm presented here uses multiple linear regression of the concentrations of one or more elements on the corrected X-ray diffraction intensities of the phases containing them. The data reduction program runs on a microcomputer. Data are presented to show its application to mineralogical analysis of artificial mixtures of quartz, microcline (a feldspar) and calcite.


2004 ◽  
Vol 834 ◽  
Author(s):  
A. V. Baryshev ◽  
T. Kodama ◽  
K. Nishimura ◽  
H. Uchida ◽  
M. Inoue

ABSTRACTWe have fabricated three-dimensional magnetophotonic (3D MPCs) crystals based on artificial opals. Structural and magnetic properties of 3D MPCs were studied by field emission scanning electron microscopy, x-ray diffraction analysis, and vibrating sample magnetometer. It was shown that increase of volume fraction of magnetite in the opal lattice leads to a dramatic decrease of transmitted light intensity in the visible region. We also found considerable changes in the Faraday rotation inside the (111) photonic bandgap of an opal—magnetite magnetophotonic crystal.


2015 ◽  
Vol 48 (3) ◽  
pp. 882-889 ◽  
Author(s):  
Jette Oddershede ◽  
Marta Majkut ◽  
Qinghua Cao ◽  
Søren Schmidt ◽  
Jonathan P. Wright ◽  
...  

A method for the extension of the three-dimensional X-ray diffraction technique to allow the extraction of domain volume fractions in polycrystalline ferroic materials is presented. This method gives access to quantitative domain volume fractions of hundreds of independent embedded grains within a bulk sample. Such information is critical to furthering our understanding of the grain-scale interactions of ferroic domains and their influence on bulk properties. The method also provides a validation tool for mesoscopic ferroic domain modelling efforts. The mathematical formulations presented here are applied to tetragonal coarse-grained Ba0.88Ca0.12Zr0.06Ti0.94O3and rhombohedral fine-grained (0.82)Bi0.5Na0.5TiO3–(0.18)Bi0.5K0.5TiO3electroceramic materials. The fitted volume fraction information is used to calculate grain-scale non-180° ferroelectric domain switching strains. The absolute errors are found to be approximately 0.01 and 0.03% for the tetragonal and rhombohedral cases, which had maximum theoretical domain switching strains of 0.47 and 0.54%, respectively. Limitations and possible extensions of the technique are discussed.


2010 ◽  
Vol 163-167 ◽  
pp. 3061-3066 ◽  
Author(s):  
Jian De Han ◽  
Gang Hua Pan ◽  
Wei Sun ◽  
Cai Hui Wang ◽  
Hui Rong

X-ray computed tomography (XCT), a non-destructive test, was used to study three dimensional (3D) meso-defect volume distribution changes of cement paste due to carbonation. The 3D meso-defect volume from 0.02mm3 ~5mm3 before and after carbonation was analyzed through add-on modules of 3D defect analysis. The experimental results show that the meso-defect volume fraction before and after carbonation are 0.7685% and 2.44%, respectively. After carbonation, the smaller defect increased significantly than the bigger defect.


2010 ◽  
Vol 44 (1) ◽  
pp. 163-171 ◽  
Author(s):  
Michelle Álvarez-Murga ◽  
Pierre Bleuet ◽  
Leonel Marques ◽  
Christophe Lepoittevin ◽  
Nathalie Boudet ◽  
...  

An extended use of synchrotron-based X-ray diffraction microtomography (XRD-µCT) to study simultaneously the phase distribution and microstructure in phase-transformation processes is proposed. This three-dimensional non-invasive imaging approach has been applied to understand the phase transformation of C60 rhombohedral polymer (C60R) into disordered graphite (DG) at high pressure and high temperature. The heterogeneous sample was synthesized (5 GPa, 1100 K) using a Paris–Edinburgh cell and selective image reconstructions were achieved for all different phases present in this sample. The XRD-µCT analysis evidences elongated DG domains with a fiber texture where nested (002)DGplanes show ±70° preferential orientation relative to the compression axis. In contrast C60R domains are found to be small and spotty, preferentially in the middle of the sample. The parent and product phases are mutually interpenetrative and exhibit a crystallographic relationship. This study evidences that formation of (002)DGplanes occurs parallel to {111}C60Cpseudo-cubic planes. Among these four possible alignments, uniaxial pressure favors one [111]C60Cdirection. Transmission electron microscopy observations validate these nondestructive XRD-µCT results.


Author(s):  
James A. Lake

The understanding of ribosome structure has advanced considerably in the last several years. Biochemists have characterized the constituent proteins and rRNA's of ribosomes. Complete sequences have been determined for some ribosomal proteins and specific antibodies have been prepared against all E. coli small subunit proteins. In addition, a number of naturally occuring systems of three dimensional ribosome crystals which are suitable for structural studies have been observed in eukaryotes. Although the crystals are, in general, too small for X-ray diffraction, their size is ideal for electron microscopy.


Author(s):  
H.W. Deckman ◽  
B.F. Flannery ◽  
J.H. Dunsmuir ◽  
K.D' Amico

We have developed a new X-ray microscope which produces complete three dimensional images of samples. The microscope operates by performing X-ray tomography with unprecedented resolution. Tomography is a non-invasive imaging technique that creates maps of the internal structure of samples from measurement of the attenuation of penetrating radiation. As conventionally practiced in medical Computed Tomography (CT), radiologists produce maps of bone and tissue structure in several planar sections that reveal features with 1mm resolution and 1% contrast. Microtomography extends the capability of CT in several ways. First, the resolution which approaches one micron, is one thousand times higher than that of the medical CT. Second, our approach acquires and analyses the data in a panoramic imaging format that directly produces three-dimensional maps in a series of contiguous stacked planes. Typical maps available today consist of three hundred planar sections each containing 512x512 pixels. Finally, and perhaps of most import scientifically, microtomography using a synchrotron X-ray source, allows us to generate maps of individual element.


2015 ◽  
Vol 71 (4) ◽  
pp. 330-337 ◽  
Author(s):  
Sabina Kovač ◽  
Ljiljana Karanović ◽  
Tamara Đorđević

Two isostructural diarsenates, SrZnAs2O7(strontium zinc diarsenate), (I), and BaCuAs2O7[barium copper(II) diarsenate], (II), have been synthesized under hydrothermal conditions and characterized by single-crystal X-ray diffraction. The three-dimensional open-framework crystal structure consists of corner-sharingM2O5(M2 = Zn or Cu) square pyramids and diarsenate (As2O7) groups. Each As2O7group shares its five corners with five differentM2O5square pyramids. The resulting framework delimits two types of tunnels aligned parallel to the [010] and [100] directions where the large divalent nine-coordinatedM1 (M1 = Sr or Ba) cations are located. The geometrical characteristics of theM1O9,M2O5and As2O7groups of known isostructural diarsenates, adopting the general formulaM1IIM2IIAs2O7(M1II= Sr, Ba, Pb;M2II= Mg, Co, Cu, Zn) and crystallizing in the space groupP21/n, are presented and discussed.


Metals ◽  
2021 ◽  
Vol 11 (5) ◽  
pp. 710
Author(s):  
Natalia Narkevich ◽  
Yevgeny Deryugin ◽  
Yury Mironov

The deformation behavior, mechanical properties, and microstructure of Fe-Cr-Mn-0.53%N austenitic stainless steel were studied at a temperature range of 77 up to 293 K. The dynamics of the steel elongation were non-monotonic with a maximum at 240–273 K, when peaks of both static atom displacements from their equilibrium positions in austenite and residual stresses in the tensile load direction were observed. The results of X-ray diffraction analysis confirmed that the only stress-induced γ→ε-martensite transformation occurred upon deformation (no traces of the γ→α′ one was found). In this case, the volume fraction of ε-martensite was about 2–3%. These transformation-induced plasticity (TRIP) patterns were discussed in terms of changes in the phase composition of steel as the root cause.


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