Elodie Boller

X-ray micro-tomography an attractive characterisation technique in materials science

X-ray tomography is a non-destructive technique which provides 3D information of materials. It is consequently very attractive in Materials Science since the relation between macroscopic properties and the micro-structure of a material is very frequently required. The aim of this paper is to present selected results obtained in various investigations of metallic materials such as superplastic deformation, materials in the semi-solid state and metallic foams. Depending on the studied features, several tomography analysis modes were used: conventional absorption mode, phase contrast and holotomography, a new technique, which provides the 3D distribution of the electron density in the bulk of the material. Furthermore micro-tomography enables one to perform in situ experiments either by using a mechanical test machine or a furnace.

In-situ deformation of an open-cell flexible polyurethane foam characterised by 3D computed microtomography

The deformation behaviour of an open-cell flexible polyurethane foam was observed using X-ray microtomography on the ID19 beamline at the ESRF in Grenoble, France. Tomographs, consisting of 1024 voxels cubed, were collected with a voxel size of 6.6 μm from a small region near the centre of the foam at a range of compressive strains between 0 and 80%. The results show that the initial stages of compression are taken up by small amounts of elastic bending in struts that are inclined to the compression direction. At 23% strain, entirely collapsed bands were observed in the structure. By 63% strain, there was evidence of struts impinging on each other, corresponding to the densification regime. The compression of an irregular foam (i.e. one with strut length and cell size distributions) appears to involve a sudden change in modulus, accompanied by localised increases in density. Observations of this nature would have been extremely difficult to interpret unambiguously without the ability to carry out sequential microtomographic imaging under realistic in situ loading conditions. The process of finite element analysis (FEA) was begun by constructing node-strut models from the experimental data by a mathematical skeletonisation process. These were used to derive node coordination, strut-length and cell-size distributions. However, direct comparison of the elastic properties with FEA was hampered by the absence of periodicity in the experimentally determined foam structures.

The Visible Cement Data Set

With advances in x-ray microtomography, it is now possible to obtain three-dimensional representations of a material’s microstructure with a voxel size of less than one micrometer. The Visible Cement Data Set represents a collection of 3-D data sets obtained using the European Synchrotron Radiation Facility in Grenoble, France in September 2000. Most of the images obtained are for hydrating portland cement pastes, with a few data sets representing hydrating Plaster of Paris and a common building brick. All of these data sets are being made available on the Visible Cement Data Set website at http://visiblecement.nist.gov. The website includes the raw 3-D datafiles, a description of the material imaged for each data set, example two-dimensional images and visualizations for each data set, and a collection of C language computer programs that will be of use in processing and analyzing the 3-D microstructural images. This paper provides the details of the experiments performed at the ESRF, the analysis procedures utilized in obtaining the data set files, and a few representative example images for each of the three materials investigated.

Three-dimensional snow images by X-ray microtomography

Abstract For the first time, three-dimensional (3-D) high-resolution images of snow were obtained using X-ray absorption tomography. Images with a spatial resolution of 10 μm were taken on four different cylindrical snow samples (9 mm high, 9 mm diameter). About 1000 two-dimensional X-ray absorption images were recorded at angular positions of the object around an axis spanning 180°. An appropriate algorithm was then used for these data to reconstruct a 3-D image. In the case of snow, experimental problems have been solved to prepare the samples and prevent both melting and metamorphism of snow during the experiments. This tomographic method provided 3-D data files from which images of 6003 voxels were extracted Several physical parameters of snow microstructure can be processed from these data. Porosity P and discrete local (3-D) curvature C of the grain/pore interface were computed for the four snow samples. Representative elementary volume (REV, in the sense of porous media) is a relevant index to the significance of the sample size with respect to a given parameter. From each image, the values of P and C are compared for subsamples of different size, as an attempt to assess the REVs for porosity and curvature. Results show that the observed volume of snow is statistically significant to achieve the porosity and the curvature distribution.

Status and evolution of the ESRF beamline ID19

The ESRF synchrotron beamline ID19, dedicated to full‐field parallel‐beam imaging techniques such as phase‐contrast and absorption microtomography and X‐ray topography, is one of the most versatile instruments of its kind. This paper presents key characteristics of ID19 in its present form, names examples for research and development performed on the beamline, and outlines the plans for an upgrade on the beamline in coming years, to adapt to the growing needs of the user community. The technical goals envisioned include an increase in available beam size and maximum photon energy, and a substantial increase in flux density for applications using beams of small and intermediate size.

Relevance of 2D radiographic texture analysis for the assessment of 3D bone micro-architecture.

Although the diagnosis of osteoporosis is mainly based on dual x-ray absorptiometry, it has been shown that trabecular bone micro-architecture is also an important factor in regard to fracture risk. In vivo, techniques based on high-resolution x-ray radiography associated to texture analysis have been proposed to investigate bone micro-architecture, but their relevance for giving pertinent 3D information is unclear. Thirty-three calcaneus and femoral neck bone samples including the cortical shells (diameter: 14mm, height: 30-40mm) were imaged using 3D-synchrotron x-ray micro-CT at the ESRF. The 3D reconstructed images with a cubic voxel size of 15μm were further used for two purposes: (1) quantification of three-dimensional trabecular bone micro-architecture, (2) simulation of realistic x-ray radiographs under different acquisition conditions. The simulated x-ray radiographs were then analyzed using a large variety of texture analysis methods (co-occurrence, spectral density, fractal, morphology, etc.). The range of micro-architecture parameters was in agreement with previous studies and rather large, suggesting that the population was representative. More than 350 texture parameters were tested. A small number of them were selected based on their correlation to micro-architectural morphometric parameters. Using this subset of texture parameters, multiple regression allowed one to predict up to 93% of the variance of micro-architecture parameters using three texture features. 2D texture features predicting 3D micro-architecture parameters other than BV/TV were identified. The methodology proposed for evaluating the relationships between 3D micro-architecture and 2D texture parameters may also be used for optimizing the conditions for radiographic imaging. Further work will include the application of the method to physical radiographs. In the future, this approach could be used in combination with DXA to refine osteoporosis diagnosis.

Nanoscale imaging of the bone cell network with synchrotron X-ray tomography: optimization of acquisition setup.

PURPOSE The fundamental role of the osteocyte cell network in regulating the bone remodeling has become evident in the last years. This has raised the necessity to explore this complex three-dimensional interconnected structure, but the existing investigation methods cannot provide an adequate assessment. The authors propose to use parallel beam synchrotron radiation computed tomography at the nanoscale to image in three dimensions the osteocyte lacunocanalicular network. To this aim, the authors study the feasibility of this technique and present an optimized imaging protocol suited for the bone cell network. Moreover, they demonstrate the multifaceted information provided by this method. METHODS The high brilliance of synchrotron radiation combined with state of art detectors permits reaching nanoscale spatial resolution. With a nominal pixel size of 280 nm, the parallel beam computed tomography setup at the ID19 experimental station of the ESRF is capable of imaging the bone lacunocanalicular network, considering that the reported diameter of canaliculi is in the range 300-600 nm. However, the actual resolution is limited by the detector and by the radiation dose causing sample damage during the scan. The authors sought to overcome these limitations by optimizing the imaging setup and the acquisition parameters in order to minimize the necessary radiation dose to create the images and to improve the spatial resolution of the detector. RESULTS The authors achieved imaging of the osteocyte cell network in human bone. Due to the optimization of the imaging setup and acquisition parameters, they obtained simultaneously a radiation dose reduction and an increase of the signal to noise ratio in the images. This permitted the authors to generate the first three-dimensional images of the lacunocanalicular network in an area covering several osteons, the fundamental functional units in the bone cortex. The method enables assessment of both architectural parameters of the microporosity and of mineralization degree in the bone matrix. The authors found that the cell network is dense and connected inside osteonal tissue. Conversely, the cell lacunae are sparse, unorganized, and disconnected in interstitial tissue. CONCLUSIONS The authors show that synchrotron radiation computed tomography is a feasible technique to assess the lacunocanalicular network in three dimensions. This is possible due to an optimal imaging setup in which the detector plays an important role. The authors could establish two valid setups, based on two different insertion devices. These results give access to new information on the bone cell network architecture, covering a number of cells two orders of magnitude greater than existing techniques. This enables biomedical studies on series of samples, paving the way to better understanding of bone fragility and to new treatments for bone diseases.

Quantitative phase contrast tomography using coherent synchrotron radiation

The coherence of third generation synchrotron beams makes a trivial form of phase-contrast imaging possible. It is based on propagation and corresponds to the defocusing technique of electron microscopy. The propagation technique can be used either in a qualitative way, mainly useful for edge- detection, or in a quantitative way, involving numerical retrieval of the phase from images recorded at different distances (typically three or four) from the sample. The combination with tomography allows to reconstruct the electron density in the sample with micrometer resolution. This combined approach is called holotomography. It was applied to several problems in materials and life sciences when it is crucial to enhance the sensitivity or reduce the dose compared to absorption tomography. Pure phase objects such as foams and fleece structures can be imaged with excellent contrast and resolution. Holotomography turned out to be a invaluable tool to study semi-solid materials with two metallurgical phases that have similar attenuation coefficients. The attenuation and density map yield in this case complementary information, the latter being the useful one to study the connectivity of the solid phase. The dose reduction and increased sensitivity in phase imaging are crucial for imaging thick (millimeter range) biological samples in their natural, wet environment. Results obtained on Arabidopsis plant indicate the possibility to investigate at the micron scale the spatial organisation of plant cells.

Slow but tenacious: an analysis of running and gripping performance in chameleons.

SUMMARY Chameleons are highly specialized and mostly arboreal lizards characterized by a suite of derived characters. The grasping feet and tail are thought to be related to the arboreal lifestyle of chameleons, yet specializations for grasping are thought to exhibit a trade-off with running ability. Indeed, previous studies have demonstrated a trade-off between running and clinging performance, with faster species being poorer clingers. Here we investigate the presence of trade-offs by measuring running and grasping performance in four species of chameleon belonging to two different clades (Chamaeleo and Bradypodion). Within each clade we selected a largely terrestrial species and a more arboreal species to test whether morphology and performance are related to habitat use. Our results show that habitat drives the evolution of morphology and performance but that some of these effects are specific to each clade. Terrestrial species in both clades show poorer grasping performance than more arboreal species and have smaller hands. Moreover, hand size best predicts gripping performance, suggesting that habitat use drives the evolution of hand morphology through its effects on performance. Arboreal species also had longer tails and better tail gripping performance. No differences in sprint speed were observed between the two Chamaeleo species. Within Bradypodion, differences in sprint speed were significant after correcting for body size, yet the arboreal species were both better sprinters and had greater clinging strength. These results suggest that previously documented trade-offs may have been caused by differences between clades (i.e. a phylogenetic effect) rather than by design conflicts between running and gripping per se.

Synchrotron 3D microtomography of halite aggregates during experimental pressure solution creep and evolution of the permeability

Pressure solution creep is one of the possible processes of mechano-chemical deformation that controls porosity and permeability variations in the upper crust. The three-dimensional geometry of the porous network of halite aggregates was imaged during compaction driven by pressure solution creep using X-ray synchrotron computed microtomography. This technique can be used to monitor individual grain contacts and whole aggregate textural changes during deformation. By reconstructing subvolumes, the 3D porosity of the aggregates was extracted. The time-resolved decrease in permeability during porosity reduction was calculated by solving the Stokes equations. The permeability remained isotropic and decreased from 2.1 to 0.15 Darcy after 18.2% compaction. Two microscopic mechanisms can explain the permeability reduction: grain indentation and pore connectivity reduction by precipitation on the free surface of pore throats.