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Do corals form their skeletons by precipitation from solution or by attachment of amorphous precursor particles as observed in other minerals and biominerals? The classical model assumes precipitation in contrast with observed "vital effects," that is, deviations from elemental and isotopic compositions at thermodynamic equilibrium. Here, we show direct spectromicroscopy evidence in Stylophora pistillata corals that two amorphous precursors exist, one hydrated and one anhydrous amorphous calcium carbonate (ACC); that these are formed in the tissue as 400-nm particles; and that they attach to the surface of coral skeletons, remain amorphous for hours, and finally, crystallize into aragonite (CaCO3). We show in both coral and synthetic aragonite spherulites that crystal growth by attachment of ACC particles is more than 100 times faster than ion-by-ion growth from solution. Fast growth provides a distinct physiological advantage to corals in the rigors of the reef, a crowded and fiercely competitive ecosystem. Corals are affected by warming-induced bleaching and postmortem dissolution, but the finding here that ACC particles are formed inside tissue may make coral skeleton formation less susceptible to ocean acidification than previously assumed. If this is how other corals form their skeletons, perhaps this is how a few corals survived past CO2 increases, such as the Paleocene-Eocene Thermal Maximum that occurred 56 Mya.

Fracture of silicon crystalline solar cells has recently been observed in increasing percentages especially in solar photovoltaic (PV) modules involving thinner silicon solar cells (

Lauretta (2005) produced sulfide in the laboratory by exposing canonical nebular metal analogs to H2S gas under temperatures and pressures relevant to the formation of the Solar System. The resulting reactions produced a suite of sulfides and nanophase materials not visible at the microprobe scale, but which we have now analyzed by TEM for comparison with interplanetary dust samples and comet Wild 2 samples returned by the Stardust mission. We find the unexpected result that disequilibrium formation favors pyrrhotite over troilite and also produces minority schreibersite, daubréelite, barringerite, taenite, oldhamite, and perryite at the metal-sulfide interface. TEM identification of nanophases and analysis of pyrrhotite superlattice reflections illuminate the formation pathway of disequilibrium sulfide. We discuss the conditions under which such disequilibrium can occur, and implications for formation of sulfide found in extraterrestrial materials.

Recently, the shape memory effect with significant recoverable shape deformation has been discovered in small volume single-crystal zirconia. The application potential for such shape memory ceramics has spurred in-depth exploration of the martensitic transformation crystallography and high temperature shape memory effect. In this work, the martensitic transformation of micron-sized zirconia has been studied in both a pristine as-produced condition and after micromechanical compression, using synchrotron scanning micro X-ray diffraction (μXRD). The pristine zirconia was found to transform into the monoclinic phase via a different crystallographic path than the compressed zirconia, resulting in distinct monoclinic variant preferences. The characteristic martensitic transformation temperatures were also found to be higher after uniaxial compression than in the pristine condition. Such observations provide insight on the differences between stress-induced and thermally-induced martensitic transformation. Moreover, we have observed a full cycle of the shape memory effect with large recoverable strain (7%) in micron-sized zirconia at a temperature of 400 °C. Our findings provide an important guideline to tailor the high-temperature shape memory properties of zirconia for further scientific research and engineering applications.

In this paper, we introduced a method to measure grain rotation of nanomaterials under external stress using a high pressure diamond anvil cell and the Laue microdiffraction technique at a synchrotron facility. We used tungsten carbide marker crystals to investigate grain rotation activities of 3 and 500 nm nickel media. Our results show that the grain rotation of 3 and 500 nm nickel nanocrystals increase with pressure and finally rotation of 500 nm nickel tends to stop at a lower pressure/stress level than 3 nm nickel. 3 nm nickel nanocrystals show a higher rotation magnitude than 500 nm nickel nanocrystals. Our measurements show an effective method to study the grain rotation of nanomaterials especially in ultrafine nanocrystals.

Ductility-dip cracking in Ni-based superalloy, resulting from heat treatment, is known to cause disastrous failure, but its mechanism is still not completely clear. A statistical study of the cracking behavior as a function of crystal orientation in a laser 3D-printed DL125L Ni-based superalloy polycrystal is investigated here using the synchrotron X-ray microdiffraction. The dislocation slip system in each of the forty crystal grains adjacent to the 300 μm long crack has been analyzed through Laue diffraction peak shapes. In all these grains, edge-type geometrically necessary dislocations (GNDs) dominate, and their dislocation line directions are almost parallel to the crack plane. Based on Schmid's law, the equivalent uniaxial tensile force direction is revealed normal to the trace of the crack. A qualitative mechanism is thus proposed. Thermal tensile stress perpendicular to the laser scanning direction is elevated due to a significant temperature gradient, and thus locations in the materials where the thermal stress exceeds the yield stress undergo plastic deformation mediated by GND activations. As the dislocations slip inside the crystal grains and pile up at the grain boundaries, local strain/stress keeps increasing, until the materials in these regions fail to sustain further deformation, leading to voids formation and cracks propagation.

Three-dimensional (3D) topological Dirac semimetals (TDSs) are rare but important as a versatile platform for exploring exotic electronic properties and topological phase transitions. A quintessential feature of TDSs is 3D Dirac fermions associated with bulk electronic states near the Fermi level. Using angle-resolved photoemission spectroscopy, we have observed such bulk Dirac cones in epitaxially grown α-Sn films on InSb(111), the first such TDS system realized in an elemental form. First-principles calculations confirm that epitaxial strain is key to the formation of the TDS phase. A phase diagram is established that connects the 3D TDS phase through a singular point of a zero-gap semimetal phase to a topological insulator phase. The nature of the Dirac cone crosses over from 3D to 2D as the film thickness is reduced.

A rotating lattice single (RLS) crystal is a unique form of solid, which was fabricated recently as one-dimensional architecture in glass via solid state transformation induced by laser irradiation. In these objects, the lattice rotates gradually and predictably about an axis that lies in the plane of the crystal and is normal to the laser scanning direction. This paper reports on the fabrication of Sb2S3 two-dimensional (2D) RLS crystals on the surface of 16SbI3-84Sb2S3 glass, as a model example: individual RLS crystal lines are joined together using "stitching" or "rastering" as two successful protocols. The electron back scattered diffraction mapping and scanning Laue X-ray microdiffraction of the 2D RLS crystals show gradual rotation of lattice comprising of two components, one along the length of each line and another normal to this direction. The former component is determined by the rotation of the first line of the 2D pattern, but the relative contribution of the last component depends on the extent of overlap between two successive lines. By the appropriate choice of initial seed orientation and the direction of scanning, it is possible to control the lattice rotation, and even to reduce it down to 5 for a 50 × 50 μm2 2D pattern of Sb2S3 crystal.

The conventional belief, based on the Read-Shockley model for the grain rotation mechanism, has been that smaller grains rotate more under stress due to the motion of grain boundary dislocations. However, in our high-pressure synchrotron Laue x-ray microdiffraction experiments, 70 nm nickel particles are found to rotate more than any other grain size. We infer that the reversal in the size dependence of the grain rotation arises from the crossover between the grain boundary dislocation-mediated and grain interior dislocation-mediated deformation mechanisms. The dislocation activities in the grain interiors are evidenced by the deformation texture of nickel nanocrystals. This new finding reshapes our view on the mechanism of grain rotation and helps us to better understand the plastic deformation of nanomaterials, particularly of the competing effects of grain boundary and grain interior dislocations.

Nacre, the iridescent outer lining of pearls and inner lining of many mollusk shells, is composed of periodic, parallel, organic sheets alternating with aragonite (CaCO3) tablet layers. Nacre tablet thickness (TT) generates both nacre's iridescence and its remarkable resistance to fracture. Despite extensive studies on how nacre forms, the mechanisms controlling TT remain unknown, even though they determine the most conspicuous of nacre's characteristics, visible even to the naked eye. Thermodynamics predicts that temperature (T) will affect both physical and chemical components of biomineralized skeletons. The chemical composition of biominerals is well-established to record environmental parameters, and has therefore been extensively used in paleoclimate studies. The physical structure, however, has been hypothesized but never directly demonstrated to depend on the environment. Here we observe that the physical TT in nacre from modern and fossil shallow-water shells of the bivalves Pinna and Atrina correlates with T as measured by the carbonate clumped isotope thermometer. Based on the observed TT vs. T correlation, we anticipate that TT will be used as a paleothermometer, useful to estimate paleotemperature in shallow-water paleoenvironments. Here we successfully test the proposed new nacre TT thermometer on two Jurassic Pinna shells. The increase of TT with T is consistent with greater aragonite growth rate at higher T, and with greater metabolic rate at higher T. Thus, it reveals a complex, T-dependent biophysical mechanism for nacre formation.

Micron-scale aluminum (Al) particles are plagued by incomplete combustion that inhibits their reactivity. One approach to improving reactivity is to anneal Al particles to increase dilatational (volumetric) strain which has also been linked to increased combustion performance. While optimal annealing temperatures have been identified (roughly 300 °C), little is known about cooling rate effects on particle combustion performance. This study examines the effect of quenching after annealing Al microparticles to 100, 200 and 300 °C on intra-particle dilatational strain and reactivity. Synchrotron X-ray diffraction analysis of the particles reveals the cooling rates in the range from 0.007 to 0.38 K/s have little effect on the dilatational strain of the aluminum-core, alumina-shell particles. The annealed and quenched Al particles were then combined with a metal oxidizer (copper oxide) to examine reactivity. Flame propagation experiments follow the same trend: flame speeds are unchanged until a critical annealing temperature of 300 °C is reached and performance is maintained for each annealing temperature regardless of cooling rate. These results show that altering the mechanical properties and combustion performance of Al particles is strongly dependent on the annealing temperature and unchanged with variation in cooling rate. The contributions from elastic and plastic deformation mechanisms on strain are also considered and additional experimental results are shown on the microstructure of an Al particle. Focused ion beam milling of an Al particle to electron transparency was combined with transmission electron microscope imaging in order to examine the microstructure of the Al particles. This confirmed that the Al microparticles have a polycrystalline structure shown by grains all exceeding 100 nm in size.

In this letter, microstructural and mechanical inhomogeneities, a great concern for single crystal Ni-based superalloys repaired by laser assisted 3D printing, have been probed near the epitaxial interface. Nanoindentation tests show the hardness to be uniformly lower in the bulk of the substrate and constantly higher in the epitaxial cladding layer. A gradient of hardness through the heat affected zone is also observed, resulting from an increase in dislocation density, as indicated by the broadening of the synchrotron X-ray Laue microdiffraction reflections. The hardening mechanism of the cladding region, on the other hand, is shown to originate not only from high dislocation density but also and more importantly from the fine γ/γ′ microstructure.

Pressure-induced phase transformation and fluorescent properties of ErF3 were investigated here using in-situ synchrotron X-ray diffraction and photoluminescence up to 32.1 GPa at room temperature. Results showed that ErF3 underwent a reversible pressure-induced phase transition from the β-YF3-type to the fluocerite LaF3-type at 9.8 GPa. The bulk moduli B0 for low- and high-pressure phases were determined to be 130 and 208 GPa, respectively. Photoluminescencent studies showed that new emission lines belonging to the transition of 2H11/2→4I15/2, 4S3/2→4I15/2, and 4F9/2→4I15/2 appeared during phase transition, suggesting pressure-induced electronic band splitting. Remarkably, significant pressure-induced enhancement of photoluminescence was observed, which was attributed to lattice distortion of the material under high pressure.

Stress relaxation in aluminum micron-scale particles covered by alumina shell after pre-stressing by thermal treatment and storage was measured using X-ray diffraction with synchrotron radiation. Pre-stressing was produced by annealing Al particles at 573K followed by fast cooling. While averaged dilatational strain in Al core was negligible for untreated particles, it was measured at 4.40×10-5 and 2.85×10-5 after 2 and 48 days of storage. Consistently, such a treatment leads to increase in flame propagation speed for Al+CuO mixture by 37% and 25%, respectively. Analytical model for creep in alumna shell and stress relaxation in Al core-alumina shell structure is developed and activation energy and pre-exponential multiplier are estimated. The effect of storage temperature and annealing temperature on the kinetics of stress relaxation was evaluated theoretically. These results provide estimates for optimizing Al reactivity with the holding time at annealing temperature and allowable time for storage of Al particles for different environmental temperatures.

Structural transformations in crystalline solids are increasingly the basis of the functional behavior of materials. Recently, in diverse alloy systems, both low hysteresis and reversibility of phase transformations have been linked to the satisfaction of the nongeneric conditions of compatibility between phases. According to the Cauchy–Born rule, these conditions are expressed as properties of transformation stretch tensor. The transformation stretch tensor is difficult to measure directly due to the lack of knowledge about the exact transforming pathway during the structural change, and the complicating effects of microstructure. In this paper we give a rigorous algorithmic approach for determining the transformation stretch tensor from X-ray measurements of structure and lattice parameters. For some traditional and emerging phase transformations, the results given by the algorithm suggest unexpected transformation mechanisms.

In this paper, a 3-D thermomechanical model of through-silicon vias (TSVs) has been analyzed and verified with in situ microscale strain measurements by synchrotron X-ray microdiffraction. Thereafter, a comprehensive stress/strain analysis on copper pumping and back-end-of-line (BEOL) cracking issues has been carried out. In addition, a design-of-experiments-based approach has been used to understand the effect of various parameters on copper pumping and BEOL stress. The results show that the smaller TSV diameter and thinner silicon die help reduce the copper pumping and thus mitigate BEOL stress.

Synchrotron-based Laue microdiffraction has been widely applied to characterize the local crystal structure, orientation, and defects of inhomogeneous polycrystalline solids by raster scanning them under a micro/nano focused polychromatic X-ray probe. In a typical experiment, a large number of Laue diffraction patterns are collected, requiring novel data reduction and analysis approaches, especially for researchers who do not have access to fast parallel computing capabilities. In this article, a novel approach is developed by plotting the distributions of the average recorded intensity and the average filtered intensity of the Laue patterns. Visualization of the characteristic microstructural features is realized in real time during data collection. As an example, this method is applied to image key features such as microcracks, carbides, heat affected zone, and dendrites in a laser assisted 3D printed Ni-based superalloy, at a speed much faster than data collection. Such analytical approach remains valid for a wide range of crystalline solids, and therefore extends the application range of the Laue microdiffraction technique to problems where real-time decision-making during experiment is crucial (for instance time-resolved non-reversible experiments).

Local crystal structure, crystal orientation, and crystal deformation can all be probed by Laue diffraction using a submicron x-ray beam. This technique, employed at a synchrotron facility, is particularly suitable for fast mapping the mechanical and microstructural properties of inhomogeneous multiphase polycrystalline samples, as well as imperfect epitaxial films or crystals. As synchrotron Laue x-ray microdiffraction enters its 20th year of existence and new synchrotron nanoprobe facilities are being built and commissioned around the world, we take the opportunity to overview current capabilities as well as the latest technical developments. Fast data collection provided by state-of-the-art area detectors and fully automated pattern indexing algorithms optimized for speed make it possible to map large portions of a sample with fine step size and obtain quantitative images of its microstructure in near real time. We extrapolate how the technique is anticipated to evolve in the near future and its potential emerging applications at a free-electron laser facility.

The alloy Cu25Au30Zn45 undergoes a huge first-order phase transformation (6% strain) and shows a high reversibility under thermal cycling and an unusual martensitc microstructure in sharp contrast to its nearby compositions. This alloy was discovered by systematically tuning the composition so that its lattice parameters satisfy the cofactor conditions (i.e., the kinematic conditions of compatibility between phases). It was conjectured that satisfaction of these conditions is responsible for the enhanced reversibility as well as the observed unusual fluid-like microstructure during transformation, but so far, there has been no direct evidence confirming that these observed microstructures are those predicted by the cofactor conditions. To verify this hypothesis, we use synchrotron X-ray Laue microdiffraction to measure the orientations and structural parameters of variants and phases near the austenite/martensite interface. The areas consisting of both austenite and multi-variants of martensite are scanned by microLaue diffraction. The cofactor conditions have been examined from the kinematic relation of lattice vectors across the interface. The continuity condition of the interface is precisely verified from the correspondent lattice vectors between two phases.

Here we report an in situ study of the early stage of microstructure evolution induced by electromigration in a Pb-free β-Sn based solder joint by synchrotron polychromatic X-ray microdiffraction. With this technique, crystal orientation evolution is monitored at intragranular levels with high spatial and angular resolution. During the entire experiment, no crystal growth is detected, and rigid grain rotation is observed only in the two grains within the current crowding region, where high density and divergence of electric current occur. Theoretical calculation indicates that the trend of electrical resistance drop still holds under the present conditions in the grain with high electrical resistivity, while the other grain with low resistivity reorients to align its a-axis more parallel with the ones of its neighboring grains. A detailed study of dislocation densities and subgrain boundaries suggests that grain rotation in β-Sn, unlike grain rotation in high melting temperature metals which undergo displacive deformation, is accomplished via diffusional process mainly, due to the high homologous temperature.

Small volume zirconia ceramics with few or no grain boundaries have been demonstrated recently to exhibit the shape memory effect. To explore the shape memory properties of yttria doped zirconia (YDZ), it is desirable to develop large, microscale grains, instead of submicron grains that result from typical processing of YDZ. In this work, we have successfully produced single crystal micro-pillars from microscale grains encouraged by the addition of titania during processing. Titania has been doped into YDZ ceramics and its effect on the grain growth, crystallization and microscale elemental distribution of the ceramics have been systematically studied. With 5 mol% titania doping, the grain size can be increased up to ~4 μm, while retaining a large quantity of the desired tetragonal phase of zirconia. Micro-pillars machined from tetragonal grains exhibit the expected shape memory effects where pillars made from titania-free YDZ would not.

We investigated the control of two important parameters of vanadium dioxide (VO2) microcrystals, the phase transition temperature and speed, by varying microcrystal width. By using the reflectivity change between insulating and metallic phases, phase transition temperature is measured by optical microscopy. As the width of square cylinder-shaped microcrystals decreases from ∼70 to ∼1 μm, the phase transition temperature (67 °C for bulk) varied as much as 26.1 °C (19.7 °C) during heating (cooling). In addition, the propagation speed of phase boundary in the microcrystal, i.e., phase transition speed, is monitored at the onset of phase transition by using the high-speed resistance measurement. The phase transition speed increases from 4.6 × 10(2) to 1.7 × 10(4) μm/s as the width decreases from ∼50 to ∼2 μm. While the statistical description for a heterogeneous nucleation process explains the size dependence on phase transition temperature of VO2, the increase of effective thermal exchange process is responsible for the enhancement of phase transition speed of small VO2 microcrystals. Our findings not only enhance the understanding of VO2 intrinsic properties but also contribute to the development of innovative electronic devices.

In bulk material processing, annealing and quenching metals such as aluminum (Al) can improve mechanical properties. On a single particle level, affecting mechanical properties may also affect Al particle reactivity. This study examines the effect of annealing and quenching on the strain of Al particles and the corresponding reactivity of aluminum and copper oxide (CuO) composites. Micron-sized Al particles were annealed and quenched according to treatments designed to affect Al mechanical properties. Synchrotron X-ray diffraction (XRD) analysis of the particles reveals that thermal treatment increased the dilatational strain of the aluminum-core, alumina-shell particles. Flame propagation experiments also show thermal treatments effect reactivity when combined with CuO. An effective annealing and quenching treatment for increasing aluminum reactivity was identified. These results show that altering the mechanical properties of Al particles affects their reactivity.

Synchrotron X-ray microdiffraction was employed to investigate the inhomogeneous distribution of defect and residual strain in the transitional region between the dendritic and stray grains in a laser-assisted 3D printed Ni-based superalloy. The dendritic region was found to be under tensile strain transversely to the primary dendrite arm directions. The dendrite edges, where high level of strains and geometrically necessary dislocations were detected, were discerned as low angle grain boundaries. High angle grain boundaries were observed in the stray grain region, and the orientation of the strain tensor in this region varied dramatically at the micron scale, in contrast with the more or less homogeneous distribution in the dendritic region.

Magnetic domain walls are boundaries between regions with different configurations of the same magnetic order. In a magnetic insulator, where the magnetic order is tied to its bulk insulating property, it has been postulated that electrical properties are drastically different along the domain walls, where the order is inevitably disturbed. Here we report the discovery of highly conductive magnetic domain walls in a magnetic insulator, Nd2Ir2O7, that has an unusual all-in-all-out magnetic order, via transport and spatially resolved microwave impedance microscopy. The domain walls have a virtually temperature-independent sheet resistance of ~1 kilohm per square, show smooth morphology with no preferred orientation, are free from pinning by disorders, and have strong thermal and magnetic field responses that agree with expectations for all-in-all-out magnetic order.

Laser additive forming is considered to be one of the promising techniques to repair single crystal Ni-based superalloy parts to extend their life and reduce the cost. Preservation of the single crystalline nature and prevention of thermal mechanical failure are two of the most essential issues for the application of this technique. Here we employ synchrotron X-ray microdiffraction to evaluate the quality in terms of crystal orientation and defect distribution of a Ni-based superalloy DZ125L directly formed by a laser additive process rooted from a single crystalline substrate of the same material. We show that a disorientation gradient caused by a high density of geometrically necessary dislocations and resultant subgrains exists in the interfacial region between the epitaxial and stray grains. This creates a potential relationship of stray grain formation and defect accumulation. The observation offers new directions on the study of performance control and reliability of the laser additive manufactured superalloys.

Archaeological artefacts are often heterogeneous materials where several phases coexist in a wide grain size distribution. Most of the time, retrieving structure information at the micrometre scale is of great importance for these materials. Particularly, the organization of different phases at the micrometre scale is closely related to optical or mechanical properties, manufacturing processes, functionalities in ancient times and long-term conservation. Between classic X-ray powder diffraction with a millimetre beam and transmission electron microscopy, a gap exists and structure and phase information at the micrometre scale are missing. Using a micrometre-size synchrotron X-ray beam, a hybrid approach combining both monochromatic powder micro-diffraction and Laue single-crystal micro-diffraction was deployed to obtain information from nanometre-and micrometre-size phases, respectively. Therefore providing a way to bridge the aforementioned gap, this unique methodology was applied to three different types of ancient materials that all show a strong heterogeneity. In Roman terra sigillata, the specific distribution of nanocrystalline hematite is mainly responsible for the deep-red tone of the slip, while the distribution of micrometre-size quartz in ceramic bodies reflects the change of manufacturing process between pre-sigillata and high-quality sigillata periods. In the second example, we investigated the modifications occurring in Neolithic and geological flints after a heating process. By separating the diffracted signal coming from the nano-and the micrometre scale, we observed a domain size increase for nanocrystalline quartz in geological flints and a relaxation of the residual strain in larger detritic quartz. Finally, through the study of a Roman iron nail, we showed that the carburation process to strengthen the steel was mainly a surface process that formed 10-20μm size domains of single-crystal ferrite and nanocrystalline cementite.

New opportunities for studying (sub)microcrystalline materials with small unit cells, both organic and inorganic, will open up when the X-ray free electron laser (XFEL) presently being constructed in Switzerland (SwissFEL) comes online in 2017. Our synchrotron-based experiments mimicking the 4%-energy-bandpass mode of the SwissFEL beam show that it will be possible to record a diffraction pattern of up to 10 randomly oriented crystals in a single snapshot, to index the resulting reflections, and to extract their intensities reliably. The crystals are destroyed with each XFEL pulse, but by combining snapshots from several sets of crystals, a complete set of data can be assembled, and crystal structures of materials that are difficult to analyze otherwise will become accessible. Even with a single shot, at least a partial analysis of the crystal structure will be possible, and with 10-50 femtosecond pulses, this offers tantalizing possibilities for time-resolved studies.

In our article, we reported the observation of monoclinic M2 to M1 structural phase transition in VO2 single crystal near the temperature of ∼49 °C. However, the re-examination of Laue patterns reveals that previously defined monoclinic M1 and M2 phases can be interpreted as monoclinic M2 and triclinic T phases instead. Careful experimental geometry calibration and further refinement of the lattice parameter ratios and angles show that monoclinic M2 and triclinic T phases fit better with the experimental data. On the other hand, our previous misidentification of the insulating phases does NOT affect the conclusions of our article.

We report on measurements of residual stress up to 300 MPa with a microfocused synchrotron X-ray beam in quartz fragments in a cataclasite from the damage zone of the San Andreas fault, California (USA). Samples were extracted from the San Andreas Fault Observatory at Depth drill core at a depth of 2.7 km. Stresses were derived from lattice distortions observed on Laue diffraction images. These stresses are distributed nonhomogeneously at the micron scale and are much higher than bulk-rock strengths of fault gouge, suggesting different processes at the microscopic and macroscopic scales. Our results indicate that residual lattice strain in quartz is a potential paleopiezometer to estimate stress in deformed rocks.

Ancient Jian wares are famous for their lustrous black glaze that exhibits unique colored patterns. Some striking examples include the brownish colored "Hare's Fur" (HF) strips and the silvery "Oil Spot" (OS) patterns. Herein, we investigated the glaze surface of HF and OS samples using a variety of characterization methods. Contrary to the commonly accepted theory, we identified the presence of ε-Fe2O3, a rare metastable polymorph of Fe2O3 with unique magnetic properties, in both HF and OS samples. We found that surface crystals of OS samples are up to several micrometers in size and exclusively made of ε-Fe2O3. Interestingly, these ε-Fe2O3 crystals on the OS sample surface are organized in a periodic two dimensional fashion. These results shed new lights on the actual mechanisms and kinetics of polymorphous transitions of Fe2O3. Deciphering technologies behind the fabrication of ancient Jian wares can thus potentially help researchers improve the ε-Fe2O3 synthesis.

Synchrotron polychromatic X-ray microdiffraction is a particularly suitable technique to study in situ the effect of electromigration in metal interconnects as add spatial resolution to grain orientation and strain sensitivity. This technique has been extensively used at the Advanced Light Source to monitor changes in aluminum and copper interconnect test structures while high-density current is passed into them during accelerated tests at elevated temperature. One of the principal findings is the observation of electromigration-induced plasticity in the metal lines that appear during the very early stages of electromigration. In some of the lines, high density of geometrically necessary dislocation are formed leading to additional diffusion paths causing an enhancement of electromigration effect at test temperature.

Wetting reaction between molten Sn-based solders and Cu produces scallop-type Cu6Sn5. In the present wetting study, a (001) single crystal Cu is used as substrate and a dramatic change in the morphology of Cu6Sn5 is observed: instead of scallop type, the authors observed a rooftop-type Cu6Sn5 grains, elongated along two preferred orientation directions. This was confirmed by electron beam backscattered diffraction and white beam synchrotron x-ray microdiffraction. The results indicate that the nucleation, growth, and ripening behavior of Cu6Sn5 on single crystal substrate can be quite different from the conventional case of wetting on randomly oriented polycrystalline Cu substrates. (14 References).

Determination of the strains in a polycrystalline material using 4-D XRD reveals sub-grain and grain-to-grain behavior as a function of stress. Here 4-D XRD involves an experimental procedure using polychromatic micro-beam X-radiation (micro-Laue) to characterize polycrystalline materials in spatial location as well as with increasing stress. The in-situ tensile loading experiment measured strain in a model aluminum-sapphire metal matrix composite using the Advanced Light Source, Beam-line 7.3.3. Micro-Laue resolves individual grains in the polycrystalline matrix. Results obtained from a list of grains sorted by crystallographic orientation depict the strain states within and among individual grains. Locating the grain positions in the plane perpendicular to the incident beam is trivial. However, determining the exact location of grains within a 3-D space is challenging. Determining the depth of the grains within the matrix (along the beam direction) involved a triangulation method tracing individual rays that produce spots on the CCD back to the point of origin. Triangulation was experimentally implemented by simulating a 3-D detector capturing multiple diffraction images while increasing the camera to sample distance. Hence by observing the intersection of rays from multiple spots belonging to the corresponding grain, depth is calculated. Depth resolution is a function of the number of images collected, grain to beam size ratio, and the pixel resolution of the CCD. The 4DXRD method provides grain morphologies, strain behavior of each grain, and interactions of the matrix grains with each other and the centrally located single crystal fiber.

The nature and proportion of Zn species present in an agricultural soil overlaid by a dredged contaminated sediment have been untangled by the novel combination of three non-invasive synchrotron-based x-ray techniques: x-ray microfluorescence ({mu}SXRF), microdiffraction ({mu}XRD), and absorption spectroscopy (EXAFS). One primary (franklinite) and two secondary (phyllomanganate and phyllosilicate) Zn-containing minerals were identified in the initial soil, and another primary (ZnS) and a new secondary (Fe-(oxyhydr)oxide) Zn species in the covered soil. The quantitative analysis of EXAFS spectra recorded on bulk samples indicated that ZnS and Zn-Fe (oxyhydr)oxides amounted to 71+-10% and 27+-10%, respectively, and the other Zn species to less than 10%. The two new Zn species found in the covered soil result from the gravitational migration of ZnS particles initially present in the sediment, and from their further oxidative dissolution and fixation of leached Zn on Fe (oxyhydr) oxides.