Quantification of fluids injection in a glass-bead matrix using X-ray microtomography

Several daily activities involve the accumulation or percolation of fluids through porous media. X-ray microtomography is a non-invasive technique capable of providing images of the internal microstructure of materials showing the different phases of fluid distribution present in the sample directly or at the pore-scale. This methodology was used to qualitatively and quantitatively assess samples consisting with glass beads of standard size, which contained fluid filling a porous region. Three samples were prepared with 0.6 mm or 0.8 mm diameter glass beads inserted into a glass tube with an inner diameter of 6.7 mm and 1.0 mm wall thickness. The fluids injected were dopant salt–water solution, industrial oil and commercial oil. The samples were scanned using a Skyscan-1172 microtomographic system. All phases present in the sample were differentiated. The values of injected fluids were determined through 2D and 3D analyses. Two types of solutions were used, one doped with KI, and the other with BaCl₂·2H₂O. The percentage of KI used allowed the individualization of the solution and, therefore, the direct quantification of this phase through 2D and 3D images.     

Accuracy evaluation of an X-ray microtomography system

Microstructural parameter evaluation of reservoir rocks is of great importance to petroleum production companies. In this connection, X-ray computed microtomography (μ-CT) has proven to be a quite useful method for the assessment of rocks, as it provides important microstructural parameters, such as porosity, permeability, pore size distribution and porous phase of the sample. X-ray computed microtomography is a non-destructive technique that enables the reuse of samples already measured and also yields 2-D cross-sectional images of the sample as well as volume rendering. This technique offers an additional advantage, as it does not require sample preparation, of reducing the measurement time, which is approximately one to three hours, depending on the spatial resolution used. Although this technique is extensively used, accuracy verification of measurements is hard to obtain because the existing calibrated samples (phantoms) have large volumes and are assessed in medical CT scanners with millimeter spatial resolution. Accordingly, this study aims to determine the accuracy of an X-ray computed microtomography system using a Skyscan 1172 X-ray microtomograph. To accomplish this investigation, it was used a nylon thread set with known appropriate diameter inserted into a glass tube. The results for porosity size and phase distribution by X-ray microtomography were very close to the geometrically calculated values. The geometrically calculated porosity and the porosity determined by the methodology using the μ-CT was 33.4 ± 3.4% and 31.0 ± 0.3%, respectively. The outcome of this investigation was excellent. It was also observed a small variability in the results along all 401 sections of the analyzed image. Minimum and maximum porosity values between the cross sections were 30.9% and 31.1%, respectively. A 3-D image representing the actual structure of the sample was also rendered from the 2-D images.     

Characterization of carbonate rocks through X-ray microfluorescence and X-ray computed microtomography

Carbonate rocks play an important role in petroleum geology by acting as reservoir rocks, generators, and even hydrocarbon sealants, accounting for about half of the oil and gas reserves known in the world. The study of these carbonate rocks have become very important in the hydrocarbon exploration scene in Brazil because of they consist in analogous for reservoir rocks of the presalt interval. Thus, the objective of this research was to use X-ray microfluorescence (micro-XRF) and X-ray microtomography analysis, as complementary techniques, in order to characterize samples of carbonate rocks in respect to their structures, textures, mineralogy, and pores. The microtomographic analyses allowed the identification of the horizontal structures as parallel lamination, horizontal, and vertical fractures filled by calcite and biotic constituents (gastropods bioclasts). Different composition of minerals were also identified, as calcite, quartz, feldspars, iron sulfides, and oxides. The porosity (ranges <1 to17%), and the high-density elements could also be quantified, as well as their distribution in each sample. The micro-XRF analysis present a direct relationship with the distribution of minerals that compound carbonate rocks, highlighting some structures, as well as helping to identify trace and minor elements in the carbonates (Mn, Sr, and Mg).     

X-ray microtomography of field-induced macro-structures in a ferrofluid

X-ray microtomography is used to visualize, in-situ, the three-dimensional nature of the magnetic field induced macro-structures (>1 μm) inside a bulk (∼1 mm diameter) magnetite-particle-mineral oil ferrofluid sample. Columnar structures of ∼10 μm diameter were seen under a 0.35 kG applied magnetic field, while labyrinth type structures ∼4 μm in width were seen at 0.55 kG. The structures have height/width aspect ratios >100. The results show that the magnetite volume fraction is not constant within the structures and on average is considerably less than a random sphere packing model.     

X-ray microtomography of 410 million-year-old optic capsules from placoderm fishes

The structure of two small ossified optic capsules from mid-Palaeozoic placoderm fishes has been revealed in fine detail, by the use of X-ray microtomography analysis and 3D visualisation software. These two specimens are 410 million-year-old; they were collected from an Early Devonian (Lochkovian) limestone in central New South Wales, and are the oldest known optic capsules from jawed fishes. The capsules show attachment areas for seven extrinsic eye muscles, rather than the six until recently deemed universal for gnathostomes. The analysis also revealed structures within the ossified cartilage which covered the medial surface of the eyeball, including nerve tracts, vascular canals, and possibly a choroid rete mirabile.     

3D quantitative image analysis of open-cell nickel foams under tension and compression loading using X-ray microtomography

The deformation behaviour and fracture of an open-cell nickel foam were analysed using X-ray microtomography at the ESRF, Grenoble, France. In situ tensile and compression tests were performed at a resolution of 2 and 10 μm. The initial morphology of the foam was studied using 3D image analysis. Parameters such as the cell volume and strut length distributions, number of faces per cell, number of nodes per face and the shape of the most representative cells were determined. The cells are shown to be non-spherical due to the initial geometrical anisotropy of the polyurethane foam template and to the load applied to the nickel foam during processing. This geometrical anisotropy is shown to be related to the observed anisotropy of the elastic properties of the material using a simple beam model. In tension, bending, stretching and alignment of struts are observed. A tensile test in the longitudinal direction is shown to reinforce the privileged orientations of the cells. In contrast, a tensile test in the transverse direction leads to a more isotropic distribution of the cells. These features are illustrated by pole figures of the three axes of equivalent ellipsoids for all cells at different strain levels. Compression tests are associated with strain localization phenomena due to the buckling of struts in a weaker region of the foam. Finally, study of open-cell nickel foam fracture shows that cracks initiate at nodes during tensile tests and that the damaged zone is about five cells wide. Free edge effects on crack initiation are also evidenced.     

Effective atomic number and density determination of rocks by X-ray microtomography

Microtomography, as a non-destructive technique, has become an important tool in studies of internal properties of materials. Recently, interest using this methodology in characterizing the samples with respect to their compositions, especially rocks, has grown. Two physical properties, density and effective atomic number, are important in determining the composition of rocks. In this work, six samples of materials with densities that varied from 2.42 to 6.84 g/cm³ and effective atomic numbers from 15.0 to 77.3 were studied. The measurements were made using a SkyScan-Bruker 1172 microtomography apparatus operating in voltages at 50, 60, 70, 80, 90 and 100 kV with a resolution of 13.1 μm. Through micro-CT images, an average gray scale was calculated for the samples and correlation studies of this value with the density and the effective atomic number of samples were made. Linear fits were obtained for each energy value. The obtained functions were tested with samples of Amazonite, Gabbro, Sandstone and Sodalite.     

Deduction of the temperature-dependent structure of the four-layer intermediate smectic phase using resonant X-ray scattering

A binary mixture of an antiferroelectric liquid-crystal material containing a selenium atom and a highly chiral dopant is investigated using resonant X-ray scattering. This mixture exhibits a remarkably wide four-layer intermediate smectic phase, the structure of which is investigated over a temperature range of 16K. Analysis of the resonant X-ray scattering data allows accurate measurement of both the helicoidal pitch and the distortion angle as a function of temperature. The former decreases rapidly as the SmC ^* phase is approached, whilst the latter remains constant over the temperature range studied at 8^°±3^° . We also observe that the senses of the helicoidal pitch and the unit cell of the repeating four-layer structure are opposite in this mixture and that there is no pitch inversion over the temperature range studied.     

Temperature evolution during scanning electron beam processing of silicon

Temperature profile evolutions produced by a scanning electron beam in crystalline silicon have been numerically calculated using a two-dimensional finite-element scheme. The temperature dependence of the different silicon properties as well as the electron penetration effects have been taken into account. Numerical calculations carried out at different conditions have been compared with experimental melting-threshold measurements using an electron beam with a Gaussian power density distribution. The good agreement between numerical calculations and experimental results proves the validity of the two-dimensional approach.     

Probing the evolution of water clusters during hydration of the solid acid catalyst H-ZSM-5

A technique developed recently for in situ solid-state ¹H NMR studies of adsorption processes has been used to probe hydration of the solid acid catalyst H-ZSM-5, yielding information on the interaction between the adsorbed water molecules and Brønsted acid sites on the H-ZSM-5 host material. Quantitative analysis of the results from the in situ experiment allows the average size of water clusters associated with the Brønsted acid sites to be determined directly, and suggests that there is a preference to form clusters comprising five–six water molecules. The in situ ¹H NMR data also provide insights into kinetic aspects of the adsorption process.     

Nano particle fluidisation in model 2-D and 3-D beds using high speed X-ray imaging and microtomography

Nanoparticles and nanocomposites have become a major focus of interest in science and technology due to exceptional properties they provide. However, handling and processing of ultra-fine powders is very challenging because they are extremely cohesive. Fluidization is one of techniques available to process powders. It has become increasingly important to understand how these nanoparticles can be handled and processed to benefit from their favourable properties. A high spatial (down to 400 nm) and temporal resolution (down to 1 ms) X-ray imaging apparatus has been designed to study nanoparticles in fluidized beds under different gas flow velocities. The mean volume distribution of the nanoparticle agglomerates was determined with X-ray microtomography. The X-ray microtomography technique provides valuable in situ, non-destructive structural information on the morphological changes that take place during fluidisation of powder samples.     

Soft X-ray absorption spectroscopy of titanium dioxide nanopowders with cobalt impurities

The charge states of the cobalt ions in TiO₂ nanopowders with the anatase lattice are studied by soft X-ray absorption spectroscopy. It is found that, at a low cobalt impurity concentration (1.8 at %), the cobalt ions with an oxidation state 2+ are mainly located in the tetrahedral (T _d ) environment of oxygen ions. Amorphous titanium dioxide exists on the sample surface before heat treatment. Annealing in vacuum or hydrogen leads to the enrichment of the nanoparticle surfaces with Co²⁺ ions, a change in the coordination of the remaining part of cobalt ions from octahedral to tetrahedral, stabilization of the anatase structure, and the disappearance of the amorphous phase. The crystal lattice of the samples with a relatively high cobalt concentration (12 at %) is distorted, and annealing does not cause the disappearance of the amorphous phase of TiO₂. Cobalt is reduced to its metallic state upon hydrogen annealing of the samples with a high cobalt concentration.     

Direct measurement of microstructural avalanches during the martensitic transition of cobalt using coherent x-ray scattering

Heterogeneous microscale dynamics in the martensitic phase transition of cobalt is investigated with real-time x-ray scattering. During the transformation of the high-temperature face-centered cubic phase to the low-temperature hexagonal close-packed phase, the structure factor evolution suggests that an initial rapid local transformation is followed by a slower period during which strain relaxes. Coherent x-ray scattering measurements performed during the latter part of the transformation show that the kinetics is dominated by discontinuous sudden changes-avalanches. The spatial size of observed avalanches varies widely, from 100 nm to 10 μm, the size of the x-ray beam. An empirical avalanche amplitude quantifies this behavior, exhibiting a power-law distribution. The avalanche rate decreases with inverse time since the onset of the transformation.     

Applications of X-ray synchrotron microtomography for non-destructive 3D studies of paleontological specimens

Paleontologists are quite recent newcomers among the users of X-ray synchrotron imaging techniques at the European Synchrotron Radiation Facility (ESRF). Studies of the external morphological characteristics of a fossil organism are not sufficient to extract all the information for a paleontological study. Nowadays observations of internal structures become increasingly important, but these observations should be non-destructive in order to preserve the important specimens. Conventional microtomography allows performing part of these investigations. Nevertheless, the best microtomographic images are obtained using third-generation synchrotrons producing hard X-rays, such as the ESRF. Firstly, monochromatisation avoids beam hardening that is frequently strong for paleontological samples. Secondly, the high beam intensity available at synchrotron radiation sources allows rapid data acquisition at very high spatial resolutions, resulting in precise mapping of the internal structures of the sample. Thirdly, high coherence leads to additional imaging possibilities: phase contrast radiography, phase contrast microtomography and holotomography. These methods greatly improve the image contrast and therefore allow studying fossils that cannot be investigated by conventional microtomography due to a high degree of mineralisation or low absorption contrast. Thanks to these different properties and imaging techniques, a synchrotron radiation source and the ESRF in particular appears as an almost ideal investigation tool for paleontology. PACS 01.30.Cc; 07.05.Hd; 68.37.Yz; 29.20.Lq; 81.70.Tx     

Radiation induced microstructural evolution and amorphization of intermetallic compounds

Abstract

A theoretical model is developed to study the influence of radiation-induced microstructural evolution on the amorphization kinetics of intermetallic compounds. The amorphization mechanism is assumed to be the buildup to a critical level of defect complexes. A complex consists of a coupled interstitial-vacancy pair. It is shown that the process of amorphization under particle bombardment is obstructed in alloy systems in which interstitials exhibit a tendency to cluster. In these systems, interstitial clustering delays the buildup of complexes. Under electron irradiation, the complex concentration attains a very low level after high doses, and the crystalline-to-amorphous transition is inhibited down to fairly low temperatures. During heavy ion bombardment, cascade damage produces an enhancement of complex formation and the transition takes place. It is shown that the kinetics of amorphization under ion bombardment depends on temperature at low temperatures, where amorphization is mostly due to complex accumulation. On the other hand, the present analyses indicate that direct in-cascade amorphization becomes more important as the bombardment temperature increases. Zr₃Al is used as a model system. The theoretical calculations yield good agreement with experimental results.     

Effect of thermomechanical processing on microstructural evolution and deformation behaviour of polycrystalline magnesium under quasi-static and high strain rate conditions

Abstract

The effect of thermomechanical processing on microstructure evolution and room temperature flow behaviour of polycrystalline magnesium in compression at strain rates of ~10^?2 and ~10³ s^?1 was investigated. Different initial microstructures were produced by optimising rolling and annealing cycles. Prior to annealing for 1 h at 350 °C, Mg samples were processed by two different treatments such as (i) hot rolling at 350 °C and (ii) hot rolling at 350 °C plus cold rolling at room temperature. Introduction of cold working step led to an increased fraction of hard oriented grains with a marginal grain size difference in post-annealed samples. A profound effect of thermomechanical processing on strain hardening rate as well as rate-sensitive flow behaviour of Mg was observed. The influence of prior processing history and strain rate on flow behaviour of Mg was clearly reflected in terms of texture strengthening/weakening phenomena and formation of microstructural deformation bands.     

Effects of heat transfer in a growing particle layer on microstructural evolution during solidification of colloidal suspensions

Heat transfer is the foundation of freezing colloidal suspensions and a key factor for the interface movement.However,how the thermal conductivity of particles affects freezing microstructural evolution remains unknown.Here in this work,a mathematical model is built up to investigate thermal interactions among a growing particle layer,pulling speeds,and the freezing interface under a thermal gradient.Experiments are conducted to confirm the tendency predictions of the model.With the increase of pulling speeds,the drifting distance of the freezing interface increases and the time to finish drifting decreases.When the thermal conductivity of particles(k_p)is smaller than that of the surrounding(kw),the freezing interface tends to go forward to the warm side.Contrarily,the freezing interface tends to go back to the cold side when the thermal conductivity of particles is larger than that of the surrounding(α=k_p/k_w>1).It originates from the shape of the local freezing interface:convex(α<1)or concave(α>1).These morphological changes in the local interface modify the premelting drag force F_f.Whenα<1,F_fdecreases and the freezing morphology tends to be the frozen fringe.Whenα>1,F_fincreases and the freezing morphologies tend to be ice spears.These understandings of how the thermal conductivity of particles affect microstructural evolution may optimize the production of freeze-casting materials and their structural-functional properties.     

冷速对液态合金Ca50Zn50快速凝固过程中微观结构演变的影响

采用分子动力学方法对六种不同冷速对原子尺寸相差较大的液态合金Ca50Znso凝固过程中微观结构演变的影响进行了模拟研究,并采用双体分布函数、Honeycutt—Andersen（HA）键型指数法、原子团类型指数法（CTIM一2）、可视化等方法进行了深入分析,结果表明：系统存在一个临界冷速,介于和5×10^11K／s与1×10^11K／s之间,在临界冷速以上（如1×10^11K／s,1×10^11K／s,1×10^11K／s和5×10^11K／s）时,系统形成以1551,1541,1431键型或二十面体基本原子团（12012000）等为主体的非晶态结构;在临界冷速以下时,系统形成以1441和1661键型或bcc基本原子团（1460800）为主体（含有少量的hcp（1200066）和fcc（12000120）基本原子团）的部分晶态结构．在非晶形成的冷速范围内,其总双体分布函数的第一峰明显分裂成与近邻分别为Zn—Zn,Ca—Zn,Ca—Ca相对应的三个次峰;且随着冷速的下降,同类原子近邻的次峰峰值升高、异类原子近邻的次峰峰值下降;Zn原子容易偏聚,随着冷速降低,二十面体的数量增多,非晶态结构也越稳定．在晶态形成的冷速范围内,Zn原子己大量偏聚形成大块bcc晶态结构,Ca原子也部分形成hcp和fcc晶态结构．     

Modelling of laser welding of flat parts using the modifying nanopowders

A mathematical model is formulated to describe thermophysical processes at laser welding of metal plates for the case when the modifying nanoparticles of refractory compounds have been introduced in the weld pool (the nanopowder seed cultrure fermenters — NSCF). Specially prepared nanoparticles of refractory compounds serve the crystallization centers that is they are in fact the exogenous primers, on the surface of which the individual clusters are grouped. Owing to this, one can control the process of the crystallization of the alloy and the formation of its structure and, consequently, the joint weld properties. As an example, we present the results of computing the butt welding of two plates of aluminum alloy and steel. Computed and experimental data are compared.     

Assessment of the fatigue crack closure phenomenon in damage-tolerant aluminium alloy by in-situ high-resolution synchrotron X-ray microtomography

Synchrotron X-ray microtomography has been utilized for the in-situ observation of steady-state plane-strain fatigue crack growth. A high-resolution experimental configuration and phase contrast imaging technique have enabled the reconstruction of crack images with an isotropic voxel with a 0.7 µm edge. The details of a crack are readily observed, together with evidence of the incidence and mechanical influence of closure. After preliminary investigations of the achievable accuracy and reproducibility, a variety of measurement methods are used to quantify crack-opening displacement (COD) and closure from the tomography data. Utilization of the physical displacements of microstructural features is proposed to obtain detailed COD data, and its feasibility is confirmed. Loss of fracture surface contact occurs gradually up to the maximum load. This is significantly different from tendencies reported where a single definable opening level is essentially assumed to exist. The closure behaviour is found to be attributable mainly to pronounced generation of mode III displacement which may be caused by local crack topology. Many small points of closure still remain near the crack tip, suggesting that the near-tip contact induces crack growth resistance. The effects of overloading are also discussed.