X-ray Refraction Research Articles

Developing a Microbubble-Based Contrast Agent for Synchrotron In-Line Phase Contrast Imaging.

X-ray phase contrast imaging generates contrast from refraction of X-rays, enhancing soft tissue contrast compared to conventional absorption-based imaging. Our goal is to develop a contrast agent for X-ray in-line phase contrast imaging (PCI) based on ultrasound microbubbles (MBs), by assessing size, shell material, and concentration. Polydisperse perfluorobutane-core lipid-shelled MBs were synthesized and size separated into five groups between 1 and 10μm. We generated two size populations of polyvinyl-alcohol (PVA)-MBs, 2-3μm and 3-4μm, whose shells were either coated or integrated with iron oxide nanoparticles (SPIONs). Microbubbles were then embedded in agar at three concentrations: 5×107, 5×106 and 5×105 MBs/ml. In-line phase contrast imaging was performed at the Canadian Light Source with filtered white beam micro-computed tomography. Phase contrast intensity was measured by both counting detectable MBs, and comparing mean pixel values (MPV) in minimum and maximum intensity projections of the overall samples. Individual lipid-MBs 6-10μm, lipid-MBs 4-6μm and PVA-MBs coated with SPIONs were detectable at each concentration. At the highest concentration, lipid-MBs 6-10μm and 4-6μm showed an overall increase in positive contrast, whereas at a moderate concentration, only lipid-MBs 6-10μm displayed an increase. Negative contrast was also observed from two largest lipid-MBs at high concentration. These data indicate that lipid-MBs larger than 4μm are candidates for PCI, and 5×106 MBs/ml may be the lowest concentration suitable for generating visible phase contrast in vivo. Identifying a suitable MB for PCI may facilitate future clinical translation.

Next-Generation Hardware Advances in CT: Cardiac Applications.

Impending major hardware advances in cardiac CT include three areas: ultra-high-resolution (UHR) CT, photon-counting CT, and phase-contrast CT. Cardiac CT is a particularly demanding CT application that requires a high degree of temporal resolution, spatial resolution, and soft-tissue contrast in a moving structure. In this review, cardiac CT is used to highlight the strengths of these technical advances. UHR CT improves visualization of calcified and stented vessels but may result in increased noise and radiation exposure. Photon-counting CT uses multiple photon energies to reduce artifacts, improve contrast resolution, and perform material decomposition. Finally, phase-contrast CT uses x-ray refraction properties to improve spatial and soft-tissue contrast. This review describes these hardware advances in CT and their relevance to cardiovascular imaging.

X-ray phase imaging reaching clinical uses.

X-ray phase imaging that uses the phenomena of X-ray refraction and scattering to generate image contrast has the potential to overcome the drawback of conventional X-ray radiography in observing biological soft tissues. After its dawn at synchrotron radiation facilities 30years ago, the development of X-ray phase imaging is expanding to hospitals by grating-based phase-imaging approaches available with a conventional X-ray tube. In this review, after introducing the physical advantages and methodological details of X-ray phase imaging, recent trials of instrumentation in hospitals for diagnoses of rheumatoid arthritis and chronic obstructive pulmonary disease are introduced.

Implementation of Talbot–Lau x-ray deflectometry in the pulsed power environment using a copper X-pinch backlighter

A Talbot–Lau x-ray deflectometer can map electron density gradients in high energy density plasmas, as well as provide information about plasma elemental composition through single-image x-ray refraction and attenuation measurements. A new adaptation to a pulsed power environment used backlighting from copper X-pinches, allowing for electron density mapping of a low-Z object. Even though the X-pinch backlighter is not properly optimized for emitting x-rays in terms of source size and photon fluence, Moire fringe patterns with contrast up to 14% and fringe shift due to refraction on a beryllium object are obtained. Due to the proximity of the deflectometer with the X-pinch (∼6 cm), it is shown that a protective filter is required to avoid damage in the closest (i.e., source) grating due to both plasma debris and mechanical shock. Regarding grating survival, these did not show any damage due to the intense magnetic field or heating induced by plasma radiation. Electron density on beryllium was measured with a difference lower than 16%. The areal electron density mapping of the sample was limited by source size characteristics, in similarity to transmission radiography. These results show the potential of plasma electron density as well as material mapping through Talbot–Lau x-ray deflectometry in a pulsed power environment.

Graphitic Nanoporous Carbon Thin Films: Fabrication Method, Structural, Electrical and Gas Sensor Properties

Carbon nanoporous thin films are very attractive for application in fields of supercapacitors, fuel cells, gas sensors and others. However due to it very high resistance an employment of this material for resistance gas sensor is problematic. At the same time graphene based materials are very sensitive to different gas ambient and have a resistivity suitable for testing. In this work the new method of formation of high porous graphite-like thin films by RF magnetron plasma enhanced chemical vapor deposition (MPECVD) from argon-methane/argon-acetylene gas mixture followed by annealing at 650ºC, is suggested. A comparative study of transformation of nanoporous carbon film produced in different carbon-hydrogen atmosphere into graphitic one, their structural and electrical properties are presented. The films of nanoporous carbon were fabricated on silicon or SiO2/Si wafers. To clarify chemical structure of the film FTIR spectroscopy and XPS were used. Micro-Raman spectroscopy and AFM were applied to determine of structure and surface morphology correspondingly. X-ray refraction (XRR) method allows us to determine a density and a thickness of the films. Four point probe method and transmittance line (TSL) technique were used for the analysis of electrical properties. Additionally, electrical conductivity at different temperature and frequency was examined by measurement of resistance between two nearest Ni contacts. The same contacts were used to estimate of the gas sensitivity.It was shown that initial deposited films have mainly sp3 C-H bonds without appearance of silicon bonds. AFM demonstrates nanostructured surface morphology with size of the surface fluctuation about 3 nm; a density of the films is about 1.3 g/cm3 for both carbon films, that corresponds to nanoporous carbon; resistivity is about 108 Ohm×cm. After thermal annealing at 650°C for 30 min in N2 atmosphere the sp3 C-H bonds are disappeared, and C=C sp2 bonds are formed. Besides the resistivity the films synthesized in argon-methane gas mixture decreases to 104 Ohm×cm whereas the films synthesized in argon-acetylene gas mixture decreases their resistivity up to 102 Ohm×cm. The density of the C films synthesized in in argon-methane gas mixture reaches about 1.5 g/cm3 that corresponds to 34% of porosity, and material shows layered structure. The density of the C films synthesized in in argon-acetylene gas mixture falls to 1.01 g/cm3 that corresponds to 55% of porosity. Graphitized films synthesized in argon-methane gas mixture appears sensory sensitivity to moisture and ammonia whereas the films synthesized in argon-acetylene gas mixture show low sensitivity to these gases. The nature of the gas sensor resistor sensitivity is discussed.

Towards Monte Carlo simulation of X-ray phase contrast using GATE.

We describe the first developments towards a Monte Carlo X-ray phase contrast imaging simulator for the medical imaging and radiotherapy simulation software GATE. Phase contrast imaging is an imaging modality taking advantage of the phase shift of X-rays. This modality produces images with a higher sensitivity than conventional, attenuation based imaging. As the first developments towards Monte Carlo phase contrast simulation, we implemented a Monte Carlo process for the refraction and total reflection of X-rays, as well as an analytical wave optics approach for generating Fresnel diffraction patterns. The implementation is validated against data acquired using a laboratory X-ray tomography system. The overall agreement between the simulations and the data is encouraging, which motivates further development of Monte Carlo based simulation of X-ray phase contrast imaging. These developments have been released in GATE version 8.2.

Experimental determination and numerical simulation of material and damage behaviour of 3D printed polyamide 12 under cyclic loading

The material and damage behaviour of additively manufactured polyamide 12 under cyclic loading was characterized by cyclic tests and microstructure analysis by using microscopy, X-ray refraction, and computed tomography. The results were used to determine parameters for the viscoplastic material model by Chaboche and a damage model by Gurson-Tvergaard-Needleman. The temperature was monitored during the experiments and the self-heating effect was observed. By including this effect, a higher accuracy could be achieved with the results of mechanical experiments.

Classification of Defect Types in SLM Ti-6Al-V4 by X-ray Refraction Topography

Abstract Porosity in additively manufactured materials, such as laser powder bed fusion Ti-Al6-V4, can play an important role in their mechanical performance. Not only the total porosity but also the shape/morphology of the individual pores need to be considered. Therefore, it is necessary to determine the distributions of different defect types (especially fusing defects and keyhole pores) and their dependence on process parameters. We show that synchrotron X-ray refraction radiography allows analysis of large samples (up to several millimeters) without compromising the detectability of submicrometer defects. Correspondingly, a classification tool is introduced that is able to quantitatively distinguish defects such as keyhole pores and binding defects with a confidence level of 94 %, even when the shape cannot be discerned because of limited spatial resolution.

Subcellular Chemical Imaging: New Avenues in Cell Biology.

To better understand the physiology and acclimation capability of the cell, one of the great challenges of the future is to access the interior of a cell and unveil its chemical landscape (composition and distribution of elements and molecules). Chemical imaging has greatly improved in sensitivity and spatial resolution to visualize and quantify nutrients, metabolites, toxic elements, and drugs in single cells at the subcellular level. This review aims to present the current potential of these emerging imaging technologies and to guide biologists towards a strategy for interrogating biological processes at the nanoscale. We also describe various solutions to combine multiple imaging techniques in a correlative way and provide perspectives and future directions for integrative subcellular imaging across different disciplines.

Drop impact on hot plates: contact times, lift-off and the lamella rupture.

When a liquid drop impacts on a heated substrate, it can remain deposited, or violently boil in contact, or lift off with or without ever touching the surface. The latter is known as the Leidenfrost effect. The duration and area of the liquid-substrate contact are highly relevant for the heat transfer, as well as other effects such as corrosion. However, most experimental studies rely on side view imaging to determine contact times, and those are often mixed with the time until the drop lifts off from the substrate. Here, we develop and validate a reliable method of contact time determination using high-speed X-ray imaging and total internal reflection imaging. We exemplarily compare contact and lift-off times on flat silicon and sapphire substrates. We show that drops can rebound even without formation of a complete vapor layer, with a wide range of lift-off times. On sapphire, we find a local minimum of lift-off times that is much shorter than expected from capillary rebound in the comparatively low-temperature regime of transition boiling/thermal atomization. We elucidate the underlying mechanism related to spontaneous rupture of the lamella and receding of the contact area.

Modern X-ray refraction optics in the course of physics of Technical University

The review of modern achievements in X-ray optics taking into account the refraction of X-rays in the matter is given. The complete external reflection of X-ray radiation from the substance allowing creating mirrors for X-ray radiation is considered. Much attention is paid to the practical use of the whispering gallery effect for X-ray radiation. An analysis of the focusing and collimation of X-ray beams by refractive lenses is given. The urgent need to include this material in the course of physics, as well as in courses on X-ray optics at Technical Universities of Russia, is noted.

The correlation between porosity characteristics and the crystallographic texture in extruded stabilized aluminium titanate for diesel particulate filter applications

Porous ceramic diesel particulate filters (DPFs) are extruded products that possess macroscopic anisotropic mechanical and thermal properties. This anisotropy is caused by both morphological features (mostly the orientation of porosity) and crystallographic texture. We systematically studied those two aspects in two aluminum titanate ceramic materials of different porosity using mercury porosimetry, gas adsorption, electron microscopy, X-ray diffraction, and X-ray refraction radiography. We found that a lower porosity content implies a larger isotropy of both the crystal texture and the porosity orientation. We also found that, analogous to cordierite, crystallites do align with their axis of negative thermal expansion along the extrusion direction. However, unlike what found for cordierite, the aluminium titanate crystallite form is such that a more pronounced (0 0 2) texture along the extrusion direction implies porosity aligned perpendicular to it.

Phase transformation induces plasticity with negligible damage in ceria-stabilized zirconia-based ceramics

Ceramics and their composites are in general brittle materials because they are predominantly made up of ionic and covalent bonds that avoid dislocation motion at room temperature. However, a remarkable ductile behavior has been observed on newly developed 11 mol.% ceria-stabilized zirconia (11Ce-TZP) composite containing fine alumina (8 vol.% Al2O3) and elongated strontium hexa-aluminate (8 vol.% SrAl12O19) grains. The as-synthesized composite also has shown full resistance to Low Temperature Degradation (LTD), relatively high strength and exceptionally high Weibull modulus, allowing its use in a broader range of biomedical applications. In this study, to deepen the understanding of plastic deformation in Ce-TZP based composites that could soon be used for manufacturing dental implants, different mechanical tests were applied on the material, followed by complete microstructural characterization. Distinct from pure Ce-TZP material or other zirconia-based ceramics developed in the past, the material here studied can be permanently strained without affecting the Young modulus, indicating that the ductile response of tested samples cannot be associated to damage occurrence. This ductility is related to the stress-induced tetragonal to monoclinic (t-m) zirconia phase transformation, analogue to Transformation-Induced Plasticity (TRIP) steels, where retained austenite is transformed to martensite. The aim of this study is to corroborate if the observed plasticity can be associated exclusively to the zirconia t-m phase transformation, or also to microcraking induced by the transformation. The t-m transformed-zones produced after bending and biaxial tests were examined by X-ray refraction and SEM/TEM coupled with Raman. The results revealed that the observed elastic-plastic behavior occurs without extensive microcracking, confirming a purely elastic-plastic behavior driven by the phase transformation (absence of damage).

Enhanced composite plate impact damage detection and characterisation using X-Ray refraction and scattering contrast combined with ultrasonic imaging

Ultrasonic imaging and radiography are widely used in the aerospace industry for non-destructive evaluation of damage in fibre-reinforced composites. Novel phase-based X-ray imaging methods use phase effects occurring in inhomogeneous specimens to extract additional information and achieve improved contrast. Edge Illumination employs a coded aperture system to extract refraction and scattering driven signals in addition to conventional absorption. Comparison with ultrasonic immersion C-scan imaging and with a commercial X-ray CT system for impact damage analysis in a small cross-ply carbon fibre-reinforced plate sample was performed to evaluate the potential of this new technique. The retrieved refraction and scattering signals provide complementary information, revealing previously unavailable insight on the damage extent and scale, not observed in the conventional X-ray absorption and ultrasonic imaging, allowing improved damage characterisation.

X-Ray Stereo Digital Image Correlation

Digital Image Correlation (DIC) is a well-established, non-contact diagnostic technique used to measure shape, displacement and strain of a solid specimen subjected to loading or deformation. However, measurements using standard DIC can have significant errors or be completely infeasible in challenging experiments, such as explosive, combustion, or fluid-structure interaction applications, where beam-steering due to index of refraction variation biases measurements or where the sample is engulfed in flames or soot. To address these challenges, we propose using X-ray imaging instead of visible light imaging for stereo-DIC, since refraction of X-rays is negligible in many situations, and X-rays can penetrate occluding material. Two methods of creating an appropriate pattern for X-ray DIC are presented, both based on adding a dense material in a random speckle pattern on top of a less-dense specimen. A standard dot-calibration target is adapted for X-ray imaging, allowing the common bundle-adjustment calibration process in commercial stereo-DIC software to be used. High-quality X-ray images with sufficient signal-to-noise ratios for DIC are obtained for aluminum specimens with thickness up to 22.2 mm, with a speckle pattern thickness of only 80 μm of tantalum. The accuracy and precision of X-ray DIC measurements are verified through simultaneous optical and X-ray stereo-DIC measurements during rigid in-plane and out-of-plane translations, where errors in the X-ray DIC displacements were approximately 2–10 μm for applied displacements up to 20 mm. Finally, a vast reduction in measurement error—5–20 times reduction of displacement error and 2–3 times reduction of strain error—is demonstrated, by comparing X-ray and optical DIC when a hot plate induced a heterogeneous index of refraction field in the air between the specimen and the imaging systems. Collectively, these results show the feasibility of using X-ray-based stereo-DIC for non-contact measurements in exacting experimental conditions, where optical DIC cannot be used.

Experimental determination and numerical simulation of material and damage behaviour of 3D printed polyamide 12 under quasi-static loading

In order to characterise the material and damage behaviour of additively manufactured polyamide 12 (PA12) under quasi-static load and to implement it in a numerical model, experiments under quasi-static load as well as microstructural investigations were carried out. Selective laser sintering (SLS) was used as the manufacturing process. For the classification of the material behaviour, quasi-static cyclic tests with holding times as well as tensile tests were performed. X-ray refraction and computed tomography (CT) were used to investigate the damage behaviour. The Chaboche model, which has already been applied for metallic materials under thermomechanical loading, served as the basis for the selection of the numerical material model. The same procedure was used for the selection of the damage model, where the Gurson–Tvergaard–Needleman (GTN) model was chosen, which was already used for porous metallic materials. The Chaboche model shows very good agreement with experimental results. Furthermore, the coupling with the GTN model allows a very good modelling of the damage behaviour. Finally, it could be shown that the selected models are suitable to simulate the material and damage behaviour of 3D printed PA12.

Diesel-induced transparency of plastically deformed high-density polyethylene

High-density polyethylene becomes optically transparent during tensile drawing when previously saturated with diesel fuel. This unusual phenomenon is investigated as it might allow conclusions with respect to the material behavior. Microscopy, differential scanning calorimetry, density measurements are applied together with two scanning X-ray scattering techniques: wide angle X-ray scattering (WAXS) and X-ray refraction, able to extract the spatially resolved crystal orientation and internal surface, respectively. The sorbed diesel softens the material and significantly alters the yielding characteristics. Although the crystallinity among stretched regions is similar, a virgin reference sample exhibits strain whitening during stretching, while the diesel-saturated sample becomes transparent. The WAXS results reveal a pronounced fiber texture in the tensile direction in the stretched region and an isotropic orientation in the unstretched region. This texture implies the formation of fibrils in the stretched region, while spherulites remain intact in the unstretched parts of the specimens. X-ray refraction reveals a preferred orientation of internal surfaces along the tensile direction in the stretched region of virgin samples, while the sample stretched in the diesel-saturated state shows no internal surfaces at all. Besides from stretching saturated samples, optical transparency is also obtained from sorbing samples in diesel after stretching.

Evolution of Thermal Microcracking in Refractory ZrO₂-SiO₂ after Application of External Loads at High Temperatures.

Zirconia-based cast refractories are widely used for glass furnace applications. Since they have to withstand harsh chemical as well as thermo-mechanical environments, internal stresses and microcracking are often present in such materials under operating conditions (sometimes in excess of 1700 °C). We studied the evolution of thermal (CTE) and mechanical (Young’s modulus) properties as a function of temperature in a fused-cast refractory containing 94 wt.% of monoclinic ZrO2 and 6 wt.% of a silicate glassy phase. With the aid of X-ray refraction techniques (yielding the internal specific surface in materials), we also monitored the evolution of microcracking as a function of thermal cycles (crossing the martensitic phase transformation around 1000 °C) under externally applied stress. We found that external compressive stress leads to a strong decrease of the internal surface per unit volume, but a tensile load has a similar (though not so strong) effect. In agreement with existing literature on β-eucryptite microcracked ceramics, we could explain these phenomena by microcrack closure in the load direction in the compression case, and by microcrack propagation (rather than microcrack nucleation) under tensile conditions.

X-ray dark-field imaging with a single absorption grating

X-ray dark-field imaging is usually performed with a Talbot–Lau interferometer, but the quality of its analyser grating is limited by the fabrication process. This makes it difficult to achieve a large area and high aspect ratio. In this study, the analyser grating is abandoned and dark-field imaging is realized using only one absorption grating. The optimal grating position is derived theoretically in the single absorption grating x-ray dark-field imaging, and the conclusion is partially verified by the experiment. Meanwhile, the optimal object position for dark-field imaging has also been obtained from both the theory and experiment. In the process of comparing x-ray dark-field imaging with x-ray refraction imaging, it is found that both of them can be explained by geometric optics, showing the intrinsic relationship between them.

Effects of impurities on the stability of the low thermal conductivity in Fe2TiO5 ceramics

The stability of the low thermal conductivity in Fe2TiO5 pseudobrookite ceramics has been studied. An increase in thermal diffusivity is observed after only three cycles of measurement. X-ray refraction shows an increase in the mean value of specific surface after the thermal diffusivity measurements. By using scanning electron microscopy and high-angle annular dark-field scanning transmission electron microscope equipped with energy dispersive X-ray spectroscopy, we observe a segregation of Ca- and F-rich nanocrystals at grain boundaries after three cycles of thermal diffusivity measurement. Therefore, impurities seem to be more efficient to scatter phonons as point defects in the pseudobrookite lattice rather than as nanocrystals at pseudobrookite grain boundaries. This emphasizes the importance of precursor purity and the influence of redistribution of impurities on thermoelectric properties: stability of micro-/nano-structures is a key point, and repeated thermoelectric measurements may allow detecting such metastable micro-/nano-structures and producing stable and reliable data.