A deformation rig for synchrotron microtomography studies of geomaterials under conditions down to 10 km depth in the Earth

A hard X‐ray transparent triaxial deformation apparatus, called HADES, has been developed by Sanchez Technologies and installed on the microtomography beamline ID19 at the European Radiation Synchrotron Facility (ESRF). This rig can be used for time‐lapse microtomography studies of the deformation of porous solids (rocks, ceramics, metallic foams) at conditions of confining pressure to 100 MPa, axial stress to 200 MPa, temperature to 250°C, and controlled aqueous fluid flow. It is transparent to high‐energy X‐rays above 60 keV and can be used for in situ studies of coupled processes that involve deformation and chemical reactions. The rig can be installed at synchrotron radiation sources able to deliver a high‐flux polychromatic beam in the hard X‐ray range to acquire tomographic data sets with a voxel size in the range 0.7–6.5 µm in less than two minutes.     

A high‐temperature furnace for in situ synchrotron X‐ray spectroscopy under controlled atmospheric conditions

A high‐temperature furnace with an induction heater coil has been designed and constructed for in situ X‐ray spectroscopic experiments under controlled atmospheric conditions and temperatures up to 3275 K. The multi‐purpose chamber design allows working in backscattering and normal fluorescence mode for synchrotron X‐ray absorption and emission spectroscopy. The use of the furnace is demonstrated in a study of the in situ formation of Cr oxide between 1823 K and 2023 K at logPO₂ values between ?10.0 and ?11.3 using X‐ray absorption near‐edge spectroscopy. The set‐up is of particular interest for studying liquid metals, alloys and other electrically conductive materials under extreme conditions.     

同步辐射X射线相衬显微CT在古生物学中的应用

X射线无损成像技术在古生物化石标本研究领域中应用十分广泛.近几年来,随着技术的不断革新,同步辐射X射线相衬显微断层成像技术(SRX-PC-μCT)也被引入到这一领域.由于同步辐射光源产生的硬X射线具有高亮度、高准直性和高空间相干性等优点,可以实现化石标本高分辨率（亚微米级）的无损三维显微成像,给古生物学的发展带来了新的机遇.文章简要回顾了用于古生物化石标本无损成像技术的发展历程,并在此基础上综述了同步辐射X射线断层显微成像技术在古生物学领域的应用现状和前景.     

Characterization of enamel caries lesions in rat molars using synchrotron X‐ray microtomography

Dental caries is a ubiquitous infectious disease with a nearly 100% lifetime prevalence. Rodent caries models are widely used to investigate the etiology, progression and potential prevention or treatment of the disease. To explore the suitability of these models for deeper investigations of intact surface zones during enamel caries, the structures of early‐stage carious lesions in rats were characterized and compared with previous reports on white spot enamel lesions in humans. Synchrotron X‐ray microcomputed tomography non‐destructively mapped demineralization in carious rat molar specimens across a range of caries severity, identifying 52 lesions across the 30 teeth imaged. Of these lesions, 13 were shown to have intact surface zones. Depth profiles of fractional mineral density were qualitatively similar to lesions in human teeth. However, the thickness of the surface zone in the rat model ranges from 10 to 58 µm, and is therefore significantly thinner than in human enamel. These results indicate that a fraction of lesions in rat caries possess an intact surface zone and are qualitatively similar to human lesions at the micrometer scale. This suggests that rat caries models may be a suitable analog through which to investigate the structure of surface zone enamel and its role during dental caries.     

Analysing the sintering of heterogeneous powder structures by in situ microtomography

This work analyses the microstructure changes of various copper-based powder systems during sintering from 3D images provided by in situ synchrotron microtomography. The investigated systems include a copper powder with a wide particle size distribution of 0–63 µm poured into a quartz capillary, a pre-sintered copper compact with artificially created large pores and a mixture of copper and alumina particles. The experiments were carried out at the European Synchrotron in Grenoble, France. Powders were sintered up to 1060°C under reducing atmosphere in a furnace located between the X-ray source and the detector. During each experiment, 3D images were taken at various times of the thermal cycle. We have obtained images with a resolution of 1.5 µm and the time of acquisition of every image was ～1 min. Quantitative analysis of these images allowed the changes of various important parameters to be followed. Such parameters characterise the sintering process at the particle length scale: interparticle coordination, pore size distribution and particle centre-to-centre distance. Moreover, by tracking the displacement of each particle centre and comparing it to the displacement predicted by classical mean field assumption, we have been able to assess the magnitude of particle rearrangement occurring during sintering. From these data, the sintering behaviour of heterogeneous powder systems is discussed with particular emphasis of collective particle phenomena.     

The contribution of synchrotron X‐ray computed microtomography to understanding volcanic processes

A series of computed microtomography experiments are reported which were performed by using a third‐generation synchrotron radiation source on volcanic rocks from various active hazardous volcanoes in Italy and other volcanic areas in the world. The applied technique allowed the internal structure of the investigated material to be accurately imaged at the micrometre scale and three‐dimensional views of the investigated samples to be produced as well as three‐dimensional quantitative measurements of textural features. The geometry of the vesicle (gas‐filled void) network in volcanic products of both basaltic and trachytic compositions were particularly focused on, as vesicle textures are directly linked to the dynamics of volcano degassing. This investigation provided novel insights into modes of gas exsolution, transport and loss in magmas that were not recognized in previous studies using solely conventional two‐dimensional imaging techniques. The results of this study are important to understanding the behaviour of volcanoes and can be combined with other geosciences disciplines to forecast their future activity.     

The 3D characteristics of post‐traumatic syringomyelia in a rat model: a propagation‐based synchrotron radiation microtomography study

Many published literature sources have described the histopathological characteristics of post‐traumatic syringomyelia (PTS). However, three‐dimensional (3D) visualization studies of PTS have been limited due to the lack of reliable 3D imaging techniques. In this study, the imaging efficiency of propagation‐based synchrotron radiation microtomography (PB‐SRµCT) was determined to detect the 3D morphology of the cavity and surrounding microvasculature network in a rat model of PTS. The rat model of PTS was established using the infinite horizon impactor to produce spinal cord injury (SCI), followed by a subarachnoid injection of kaolin to produce arachnoiditis. PB‐SRµCT imaging and histological examination, as well as fluorescence staining, were conducted on the animals at the tenth week after SCI. The 3D morphology of the cystic cavity was vividly visualized using PB‐SRµCT imaging. The quantitative parameters analyzed by PB‐SRµCT, including the lesion and spared spinal cord tissue area, the minimum and maximum diameters in the cystic cavity, and cavity volume, were largely consistent with the results of the histological assessment. Moreover, the 3D morphology of the cavity and surrounding angioarchitecture could be simultaneously detected on the PB‐SRµCT images. This study demonstrated that high‐resolution PB‐SRµCT could be used for the 3D visualization of trauma‐induced spinal cord cavities and provides valuable quantitative data for cavity characterization. PB‐SRµCT could be used as a reliable imaging technique and offers a novel platform for tracking cavity formation and morphological changes in an experimental animal model of PTS.     

Similarities and differences in radiation damage at 100 K versus 160 K in a crystal of thermolysin

The temperature‐dependence of radiation damage in macromolecular X‐ray crystallography is currently much debated. Most protein crystallographic studies are based on data collected at 100 K. Data collection at temperatures below 100 K has been proposed to reduce radiation damage and above 100 K to be useful for kinetic crystallography that is aimed at the generation and trapping of protein intermediate states. Here the global and specific synchrotron‐radiation sensitivity of crystalline thermolysin at 100 and 160 K are compared. Both types of damage are higher at 160 K than at 100 K. At 160 K more residue types are affected (Lys, Asp, Gln, Pro, Thr, Met, Asn) than at 100 K (Met, Asp, Glu, Lys). The X‐ray‐induced relative atomic B‐factor increase is shown to correlate with the proximity of the atom to the nearest solvent channel at 160 K. Two models may explain the observed correlation: either an increase in static disorder or an increased attack of hydroxyl radicals from the solvent area of the crystal.     

A scanning Kelvin probe for synchrotron investigations: the in situ detection of radiation‐induced potential changes

A wide range of high‐performance X‐ray surface/interface characterization techniques are implemented nowadays at every synchrotron radiation source. However, these techniques are not always `non‐destructive' because possible beam‐induced electronic or structural changes may occur during X‐ray irradiation. As these changes may be at least partially reversible, an in situ technique is required for assessing their extent. Here the integration of a scanning Kelvin probe (SKP) set‐up with a synchrotron hard X‐ray interface scattering instrument for the in situ detection of work function variations resulting from X‐ray irradiation is reported. First results, obtained on bare sapphire and sapphire covered by a room‐temperature ionic liquid, are presented. In both cases a potential change was detected, which decayed and vanished after switching off the X‐ray beam. This demonstrates the usefulness of a SKP for in situ monitoring of surface/interface potentials during X‐ray materials characterization experiments.     

A low‐cost X‐ray‐transparent experimental cell for synchrotron‐based X‐ray microtomography studies under geological reservoir conditions

A new modular X‐ray‐transparent experimental cell enables tomographic investigations of fluid rock interaction under natural reservoir conditions (confining pressure up to 20 MPa, pore fluid pressure up to 15 MPa, temperature ranging from 296 to 473 K). The portable cell can be used at synchrotron radiation sources that deliver a minimum X‐ray flux density of 10⁹ photons mm^?2 s^?1 in the energy range 30–100 keV to acquire tomographic datasets in less than 60 s. It has been successfully used in three experiments at the bending‐magnet beamline 2BM at the Advanced Photon Source. The cell can be easily machined and assembled from off‐the‐shelf components at relatively low costs, and its modular design allows it to be adapted to a wide range of experiments and lower‐energy X‐ray sources.     

Photoluminescence in γ-irradiated α-quartz investigated by synchrotron radiation

We report an experimental investigation of the photoluminescence, under excitation by synchrotron radiation within the absorption band at 7.6 eV, induced in γ-irradiated α-quartz. Two emissions centered at 4.9 and 2.7 eV are observed at low temperature: the former decreases above 40 K, whereas the second band exhibits an initial slight increase and its quenching is effective above 100 K. Furthermore, the decay kinetics of both emissions occur in a time scale of nanoseconds: at T=17.5 K we measured a lifetime τ1.0 ns for the photoluminescence at 4.9 eV and τ3.6 ns for that at 2.7 eV. These results give new insight on the optical properties associated with defects peculiar of crystalline matrix, also on the basis of their comparison with previous studies on silica.     

同步辐射光源的反馈控制模型

同步辐射光源的不稳定性是客观存在的问题,产生不稳定性的原因很多。对系统中客观存在的物理现象进行了讨论,提出了一些解决问题的方法,特别是反馈控制。同步辐射加速器反馈控制是一个比较复杂的问题,它涉及到高能电子束团在相空间的稳定运动。在实际应用中,存在一些反馈系统在一定程度上改善了同步辐射光源的稳定性,对实际应用于同步辐射装置的反馈系统进行了分析,提出了适合于同步辐射光源的反馈控制模型。     

Nondestructive imaging of the internal microstructure of vessels and nerve fibers in rat spinal cord using phase‐contrast synchrotron radiation microtomography

The spinal cord is the primary neurological link between the brain and other parts of the body, but unlike those of the brain, advances in spinal cord imaging have been challenged by the more complicated and inhomogeneous anatomy of the spine. Fortunately with the advancement of high technology, phase‐contrast synchrotron radiation microtomography has become widespread in scientific research because of its ability to generate high‐quality and high‐resolution images. In this study, this method has been employed for nondestructive imaging of the internal microstructure of rat spinal cord. Furthermore, digital virtual slices based on phase‐contrast synchrotron radiation were compared with conventional histological sections. The three‐dimensional internal microstructure of the intramedullary arteries and nerve fibers was vividly detected within the same spinal cord specimen without the application of a stain or contrast agent or sectioning. With the aid of image post‐processing, an optimization of vessel and nerve fiber images was obtained. The findings indicated that phase‐contrast synchrotron radiation microtomography is unique in the field of three‐dimensional imaging and sets novel standards for pathophysiological investigations in various neurovascular diseases.     

Intracerebral delivery of 5‐iodo‐2′‐deoxyuridine in combination with synchrotron stereotactic radiation for the therapy of the F98 glioma

Iodine‐enhanced synchrotron stereotactic radiotherapy takes advantage of the radiation dose‐enhancement produced by high‐Z elements when irradiated with mono‐energetic beams of synchrotron X‐rays. In this study it has been investigated whether therapeutic efficacy could be improved using a thymidine analogue, 5‐iodo‐2′‐deoxyuridine (IUdR), as a radiosentizing agent. IUdR was administered intracerebrally over six days to F98 glioma‐bearing rats using Alzet osmotic pumps, beginning seven days after tumor implantation. On the 14th day, a single 15 Gy dose of 50 keV synchrotron X‐rays was delivered to the brain. Animals were followed until the time of death and the primary endpoints of this study were the mean and median survival times. The median survival times for irradiation alone, chemotherapy alone or their combination were 44, 32 and 46 days, respectively, compared with 24 days for untreated controls. Each treatment alone significantly increased the rats' survival in comparison with the untreated group. Their combination did not, however, significantly improve survival compared with that of X‐irradiation alone or chemotherapy alone. Further studies are required to understand why the combination of chemoradiotherapy was no more effective than X‐irradiation alone.     

A simple polarimeter for quantifying synchrotron polarization

There are currently no simple and easy to apply techniques for determining the degree of linear polarization of a soft X-ray beam delivered by a synchrotron beamline despite the fact that this parameter is important for a wide range of synchrotron-based soft X-ray experiments. This work presents a new method for the quantitative determination of the linear polarization state of synchrotron radiation using an HOPG crystal as the standard sample. The method is straightforward to perform without the need for experimental apparatus beyond that commonly available at beamlines in this energy range. In addition, the high-degree of order that can easily be achieved in a HOPG sample means that it is potentially more accurate than currently employed comparative methods. We show how the method can be applied to experimentally determine the linear polarization state of various soft X-ray synchrotron beamlines and we discuss the wide variations in the degree of linear polarization that are measured.     

Numerical modelling of heat transfer in plasma shaft electric furnace at utilization of anthropogenic waste

The mathematical model of heat transfer between the counter flows of gas and porous batch of anthropogenic wastes in the working area of a shaft furnace is presented. This model considers chemical transformations in separate batch components and radiation heat transfer between the gas and solid phases. Results of calculations are presented.     

同步辐射成像技术在材料科学中的应用——金属合金晶体生长原位可视化

金属及其合金是一类重要的结构和功能材料,广泛应用于航空航天、汽车、造船等行业.金属合金的宏观性能实质上取决于其微观组织,微观组织的演变通常是一个微米范畴的晶体生长过程.由于金属合金的不透明性以及结晶过程的高温环境,长期以来,金属合金的晶体生长过程如同一个黑匣子,一直不为人们所知,只能通过分析最终微观组织或者中间淬火组织来推断黑匣子里可能发生了哪些现象.同步辐射X射线实时成像技术的出现,为实现金属合金晶体生长的原位可视化提供了可能,从而找到了打开这一黑匣子的钥匙.文章介绍了金属合金晶体生长原位可视化研究工作的发展历程及最新进展,列举了应用同步辐射实时成像技术原位观察合金晶体生长行为的典型研究结果,并对该成像技术在金属材料领域的未来应用进行了展望.     

Determination of Zn distribution and speciation in basic oxygen furnace sludge by synchrotron radiation induced μ‐XRF and μ‐XANES microspectroscopy

Basic oxygen furnace off gas (BOF OG) sludge is one important type of metallurgical residues in steelmaking industry. The presence of zinc element is one key factor that constrains the practical use of such metallurgical residues. Information about the chemical association of zinc in BOF OG sludge is fundamental for understanding its behavior during the formation and further treatments. In this paper, the spatial distribution and the chemical forms of zinc in accumulated particles of BOF OG sludge have been investigated using synchrotron radiation induced μ‐X‐ray fluorescence and μ‐X‐ray absorption near edge spectroscopy microspectroscopy. Results of μ‐X‐ray fluorescence analysis showed that zinc distributed in two ways. One was shared with iron, and its distribution showed a positive correlation with that of iron. The other was accumulated in some well‐defined hot spots with high amount and its distribution showed negative correlation with that of iron. And results of μ‐X‐ray absorption near edge spectroscopy microspectroscopy indicated that ZnFe₂O₄ was the main constituent in some well‐defined hot spots, whereas in other cases, zinc was mainly in the form of zinc carbonate. Copyright © 2013 John Wiley & Sons, Ltd.     

A nearly zero temperature gradient furnace system for high pressure multi-anvil experiments

A new furnace system with an almost zero temperature gradient throughout the sample area was designed for multi-anvil high pressure experiments. Test experiments of the new design were performed using 18/11 and 25/15 cell assemblies at 4?GPa, 1400°C and 1500°C, respectively. The temperature field within the sample capsules appeared to be very homogenous as indicated by Mg₂Si₂O₆–MgCaSi₂O₆ two-pyroxene thermometry, by direct temperature measurements using two thermocouples within the same assembly, and by distribution of solid and liquid phases in the sample capsule. The temperature gradient is estimated to be <2.4°C/mm over an area of 4?×?5?mm² within the furnace. It is significantly lower than standard multi-anvil experiments with straight or stepped furnace systems, which are at the levels of 20–200°C/mm.     

Performance of the far‐IR beamline of the 6 MeV tabletop synchrotron light source

The performance of the far‐infrared (FIR) beamline of the 6 MeV tabletop synchrotron light source MIRRORCLE‐6FIR dedicated to far‐infrared spectroscopy is presented. MIRRORCLE‐6FIR is equipped with a perfectly circular optical system (PhSR) placed around the 1 m‐long circumference electron orbit. To illustrate the facility of this light source, the FIR output as well as its spectra were measured. The optimum optical system was designed by using the ray‐tracing simulation code ZEMAX. The measured FIR intensity with the PhSR in place is about five times higher than that without the PhSR, which is in good agreement with the simulation results. The MIRRORCLE‐6FIR spectral flux is compared with a standard thermal source and is found to be 1000 times greater than that from a typical thermal source at ～15 cm^?1. It is also observed that the MIRRORCLE‐6FIR radiation has a highly coherent nature. The broadband infrared allows the facility to reach the spectral range from 10 cm^?1 to 100 cm^?1. MIRRORCLE‐6FIR, owing to a large beam current, the PhSR mirror system, a large dynamic aperture and small ring energy, can deliver a bright flux of photons in the FIR/THz region useful for broadband spectroscopy.