M. Di Michiel

Morphological clues to wet granular pile stability

When a granular material such as sand is mixed with a certain amount of liquid, the surface tension of the latter bestows considerable stiffness to the material, which enables, for example, sand castles to be sculpted. The geometry of the liquid interface within the granular pile is of extraordinary complexity and strongly varies with the liquid content. Surprisingly, the mechanical properties of the pile are largely independent of the amount of liquid over a wide range. We resolve this puzzle with the help of X-ray microtomography, showing that the remarkable insensitivity of the mechanical properties to the liquid content is due to the particular organization of the liquid in the pile into open structures. For spherical grains, a simple geometric rule is established, which relates the macroscopic properties to the internal liquid morphologies. We present evidence that this concept is also valid for systems with non-spherical grains. Hence, our results provide new insight towards understanding the complex physics of a large variety of wet granular systems including land slides, as well as mixing and agglomeration problems.

On the implementation of computed laminography using synchrotron radiation

Hard x rays from a synchrotron source are used in this implementation of computed laminography for three-dimensional (3D) imaging of flat, laterally extended objects. Due to outstanding properties of synchrotron light, high spatial resolution down to the micrometer scale can be attained, even for specimens having lateral dimensions of several decimeters. Operating either with a monochromatic or with a white synchrotron beam, the method can be optimized to attain high sensitivity or considerable inspection throughput in synchrotron user and small-batch industrial experiments. The article describes the details of experimental setups, alignment procedures, and the underlying reconstruction principles. Imaging of interconnections in flip-chip and wire-bonded devices illustrates the peculiarities of the method compared to its alternatives and demonstrates the wide application potential for the 3D inspection and quality assessment in microsystem technology.

Dynamic X‐Ray Diffraction Computed Tomography Reveals Real‐Time Insight into Catalyst Active Phase Evolution

Metals and metal oxides anchored to porous support materials are widely used as heterogeneous catalysts in a number of important industrial chemical processes. These catalysts owe their activity to the formation of unique metal/metal oxide support interactions, typically resulting in highly dispersed actives stabilized in a particular electronic or coordination state. They are employed in fixed-bed reactors as extruded or pelletized millimeter-sized “catalyst bodies” minimizing pressure drops along the length of the reactor. Since the efficiency of the whole catalytic system depends on the behavior and efficiency of the catalyst body per se, its design has very great importance. Crucial to this design is an understanding of the factors which influence the distribution and nature of the active phase during preparation. The type of desired distribution is very much dependant on catalytic process and required products; for example, an egg-shell distribution (as opposed to uniform, egg-white, or egg-yolk), where the active phase is located at the edges of the catalyst body, can be favored if the product forms readily.

Bubble formation within filaments of melt-processed Bi2212 wires and its strongly negative effect on the critical current density

Most studies of Bi2Sr2CaCu2Ox (Bi2212) show that the critical current density Jc is limited by the connectivity of the filaments, but what determines the connectivity is still elusive. Here we report on the role played by filament porosity in limiting Jc. By a microstructural investigation of wires quenched from the melt state, we find that porosity in the unreacted wire agglomerates into bubbles that segment the Bi2212 melt within the filaments into discrete sections. These bubbles do not disappear during subsequent processing because they are only partially filled by Bi2212 grains as the Bi2212 forms on cooling. Correlating the microstructure of quenched wires to their final, fully processed Jc values shows an inverse relation between Jc and bubble density. Bubbles are variable between conductors and perhaps from sample to sample, but they occur frequently and almost completely fill the filament diameter, so they exert a strongly variable but always negative effect on Jc. Bubbles reduce the continuous Bi2212 path within each filament and force supercurrent to flow through Bi2212 grains that span the bubbles or through a thin Bi2212 layer at the interface between the bubble and the Ag matrix. Eliminating bubbles appears to be a promising new path to raise the Jc of Bi2212 round wires.

Fast processes in liquid metal foams investigated by high-speed synchrotron x-ray microradioscopy

Rupture of an individual film in an evolving liquid metal foam is investigated by means of high-speed x-ray radioscopy using white synchrotron radiation. At a frame rate of 5000frames∕s, the rupture event is spread over three to four images. The images show that the remnants of the rupturing film are pulled into the surrounding plateau borders in 600±100μs which conforms well with a liquid movement governed by inertia and not by viscosity. Within one order of magnitude, the viscosity of the liquid involved must be similar to the viscosity of pure liquid aluminium.

Time-lapse, three-dimensional in situ imaging of ice crystal growth in a colloidal silica suspension

Abstract The freezing of colloidal suspensions is encountered in many natural and engineering processes such as the freezing of soils, food engineering and cryobiology. It can also be used as a bio-inspired, versatile and environmentally friendly processing route for porous materials and composites. Yet, it is still a puzzling phenomenon with many unexplained features, owing to the complexity of the system and the space and time scales at which the process should be investigated. This study demonstrates the interest in fast X-ray computed tomography for providing time-lapse, three-dimensional, in situ imaging of ice crystal growth in a colloidal silica suspension. The experimental measurements show that the local increase in colloid concentration does not affect the growth kinetics of the crystals until the colloidal particles become closely packed. For particles much smaller than ice crystals, the concentrated colloidal suspension is equivalent to a simple liquid phase with higher viscosity and a freezing point determined by the concentration of colloidal particles.

Liquid distribution and cohesion in wet granular assemblies beyond the capillary bridge regime

Dry sand turns into a stiff and moldable material as soon as it is mixed with some liquid. This is a direct consequence of the internal liquid–air interfaces spanning between the grains which causes capillary cohesion by virtue of the surface tension of the liquid. As a model for wet granulates we investigated random packings of submillimeter spherical beads mixed with water. Measurements of the tensile strength and the fluidization threshold demonstrate that the mechanical stiffness is rather insensitive to the liquid content over a wide range. Only for a high liquid content, when more than half of the available pore space is filled with liquid, does the capillary cohesion weaken. In order to understand the interplay between the mechanical properties and the liquid content, we investigated the liquid distribution in random packings of glass spheres by means of x-ray microtomography. The three-dimensional images reveal that the liquid forms a network of capillary bridges fused at local triangular bead configurations. The spontaneous organization of the liquid into these ramified structures, which exhibit a large liquid–air interface, is responsible for the constancy of the cohesive forces in a wide range of liquid contents beyond the onset of capillary bridge coalescence.

Reduction of Gas Bubbles and Improved Critical Current Density in Bi-2212 Round Wire by Swaging

Bi-2212 round wire is made by the powder-in-tube technique. An unavoidable property of powder-in-tube conductors is that there is about 30% void space in the as-drawn wire. We have recently shown that the gas present in the as-drawn Bi-2212 wire agglomerates into large bubbles and that they are presently the most deleterious current-limiting mechanism. By densifying short 2212 wires before reaction through cold isostatic pressing, the void space was almost removed and the gas bubble density was reduced significantly, resulting in a doubled engineering critical current density (JE) of 810 A/mm2 at 5 T, 4.2 K. Here we report on densifying Bi-2212 wire by swaging, which increased JE (4.2 K, 5 T) from 486 A/mm2 for as-drawn wire to 808 A/mm2 for swaged wire. This result further confirms that enhancing the filament packing density is of great importance for making major JE improvements in this round-wire magnet conductor.

Void and phase evolution during the processing of Bi-2212 superconducting wires monitored by combined fast synchrotron micro-tomography and x-ray diffraction

Recent study of the current-limiting mechanisms in Bi-2212 round wires has suggested that agglomeration of the residual Bi-2212 powder porosity into bubbles of filament-diameter size occurs on melting the Bi-2212 filaments. These pores introduce a major obstacle to current flow, which greatly reduces the critical current density (Jc). Here we present an in situ non-destructive tomographic and diffraction study of the changes occurring during the heat treatment of wires and starting powder, as well as a room temperature study of ex situ processed wires. The in situ through-process study shows that the agglomeration of residual porosity is more complex than previously seen. Filament changes start with coalescence of the quasi-uniform and finely divided powder porosity into lens-shaped defects at about 850 °C when the Bi-2201 impurity phase decomposes before the Bi-2212 starts to melt. These lens-shaped voids grow to bubbles of a filament diameter on melting of the Bi-2212 and continue to lengthen and then to agglomerate across multiple filaments while the filaments are in the liquid state. The experiment makes clear why melt processing is vital to developing high Jc and also shows how rearrangement of the residual filament porosity on melting imposes a strong longitudinal inhomogeneity in each filament. Reducing the bubble density is clearly an important path to reaching much higher Jc values in Bi-2212 round wires. Synchrotron micro-tomography is an exceptionally powerful technique for studying the spatial extent of the porosity on a scale of about 2 µm and larger.

Evidence for length-dependent wire expansion, filament dedensification and consequent degradation of critical current density in Ag-alloy sheathed Bi-2212 wires

It is well known that longer Bi-2212 conductors have significantly lower critical current density (Jc) than shorter ones, and recently it has become clear that a major cause of this reduction is internal gas pressure generated during heat treatment, which expands the wire diameter and dedensifies the Bi-2212 filaments. Here we report on the length-dependent expansion of 5–240 cm lengths of state-of-the-art, commercial Ag alloy sheathed Bi-2212 wire after full and some partial heat treatments. Detailed image analysis along the wire length shows that the wire diameter increases with distance from the ends, longer samples often showing evident damage and leaks provoked by the internal gas pressure. Comparison of heat treatments carried out just below the melting point and with the usual melt process makes it clear that melting is crucial to developing high internal pressure. The decay of Jc away from the ends is directly correlated to the local wire diameter increase, which decreases the local Bi-2212 filament mass density and lowers Jc, often by well over 50%. It is clear that control of the internal gas pressure is crucial to attaining the full Jc of these very promising round wires and that the very variable properties of Bi-2212 wires are due to the fact that this internal gas pressure has so far not been well controlled.