Release dynamics of nanodiamonds created by laser-driven shock-compression of polyethylene terephthalate.

Laser-driven dynamic compression experiments of plastic materials have found surprisingly fast formation of nanodiamonds (ND) via X-ray probing. This mechanism is relevant for planetary models, but could also open efficient synthesis routes for tailored NDs. We investigate the release mechanics of compressed NDs by molecular dynamics simulation of the isotropic expansion of finite size diamond from different P-T states. Analysing the structural integrity along different release paths via molecular dynamic simulations, we found substantial disintegration rates upon shock release, increasing with the on-Hugnoiot shock temperature. We also find that recrystallization can occur after the expansion and hence during the release, depending on subsequent cooling mechanisms. Our study suggests higher ND recovery rates from off-Hugoniot states, e.g., via double-shocks, due to faster cooling. Laser-driven shock compression experiments of polyethylene terephthalate (PET) samples with in situ X-ray probing at the simulated conditions found diamond signal that persists up to 11 ns after breakout. In the diffraction pattern, we observed peak shifts, which we attribute to thermal expansion of the NDs and thus a total release of pressure, which indicates the stability of the released NDs.

Pore evolution mechanisms during directed energy deposition additive manufacturing.

Porosity in directed energy deposition (DED) deteriorates mechanical performances of components, limiting safety-critical applications. However, how pores arise and evolve in DED remains unclear. Here, we reveal pore evolution mechanisms during DED using in situ X-ray imaging and multi-physics modelling. We quantify five mechanisms contributing to pore formation, migration, pushing, growth, removal and entrapment: (i) bubbles from gas atomised powder enter the melt pool, and then migrate circularly or laterally; (ii) small bubbles can escape from the pool surface, or coalesce into larger bubbles, or be entrapped by solidification fronts; (iii) larger coalesced bubbles can remain in the pool for long periods, pushed by the solid/liquid interface; (iv) Marangoni surface shear flow overcomes buoyancy, keeping larger bubbles from popping out; and (v) once large bubbles reach critical sizes they escape from the pool surface or are trapped in DED tracks. These mechanisms can guide the development of pore minimisation strategies.

Development towards high-resolution kHz-speed rotation-free volumetric imaging.

X-ray multi-projection imaging (XMPI) has the potential to provide rotation-free 3D movies of optically opaque samples. The absence of rotation enables superior imaging speed and preserves fragile sample dynamics by avoiding the centrifugal forces introduced by conventional rotary tomography. Here, we present our XMPI observations at the ID19 beamline (ESRF, France) of 3D dynamics in melted aluminum with 1000 frames per second and 8 µm resolution per projection using the full dynamical range of our detectors. Since XMPI is a method under development, we also provide different tests for the instrumentation of up to 3000 frames per second. As the high-brilliance of 4th generation light-sources becomes more available, XMPI is a promising technique for current and future X-ray imaging instruments.

Multiscale drainage dynamics with Haines jumps monitored by stroboscopic 4D X-ray microscopy.

Slow multiphase flow in porous media is intriguing because its underlying dynamics is almost deterministic, yet depends on a hierarchy of spatiotemporal processes. There has been great progress in the experimental study of such multiphase flows, but three-dimensional (3D) microscopy methods probing the pore-scale fluid dynamics with millisecond resolution have been lacking. Yet, it is precisely at these length and time scales that the crucial pore-filling events known as Haines jumps take place. Here, we report four-dimensional (4D) (3D + time) observations of multiphase flow in a consolidated porous medium as captured in situ by stroboscopic X-ray micro-tomography. With a total duration of 6.5 s and 2 kHz frame rate, our experiments provide unprecedented access to the multiscale liquid dynamics. Our tomography strategy relies on the fact that Haines jumps, although irregularly spaced in time, are almost deterministic, and therefore repeatable during imbibition-drainage cycling. We studied the time-dependent flow pattern in a porous medium consisting of sintered glass shards. Exploiting the repeatability, we could combine the radiographic projections recorded under different angles during successive cycles into a 3D movie, allowing us to reconstruct pore-scale events, such as Haines jumps, with a spatiotemporal resolution that is two orders of magnitude higher than was hitherto possible. This high resolution allows us to explore the detailed interfacial dynamics during drainage, including fluid-front displacements and velocities. Our experimental approach opens the way to the study of fast, yet deterministic mesoscopic processes also other than flow in porous media.

Cavitation cloud formation and surface damage of a model stone in a high-intensity focused ultrasound field.

This work investigates the fundamental role of cavitation bubble clouds in stone comminution by focused ultrasound. The fragmentation of stones by ultrasound has applications in medical lithotripsy for the comminution of kidney stones or gall stones, where their fragmentation is believed to result from the high acoustic wave energy as well as the formation of cavitation. Cavitation is known to contribute to erosion and to cause damage away from the target, yet the exact contribution and mechanisms of cavitation remain currently unclear. Based on in situ experimental observations, post-exposure microtomography and acoustic simulations, the present work sheds light on the fundamental role of cavitation bubbles in the stone surface fragmentation by correlating the detected damage to the observed bubble activity. Our results show that not all clouds erode the stone, but only those located in preferential nucleation sites whose locations are herein examined. Furthermore, quantitative characterizations of the bubble clouds and their trajectories within the ultrasonic field are discussed. These include experiments with and without the presence of a model stone in the acoustic path length. Finally, the optimal stone-to-source distance maximizing the cavitation-induced surface damage area has been determined. Assuming the pressure magnitude within the focal region to exceed the cavitation pressure threshold, this location does not correspond to the acoustic focus, where the pressure is maximal, but rather to the region where the acoustic beam and thereby the acoustic cavitation activity near the stone surface is the widest.

Synchrotron-based x ray fluorescence ghost imaging.

X ray fluorescence ghost imaging (XRF-GI) was recently demonstrated for x ray lab sources. It has the potential to reduce the acquisition time and deposited dose by choosing their trade-off with a spatial resolution while alleviating the focusing constraints of the probing beam. Here, we demonstrate the realization of synchrotron-based XRF-GI: we present both an adapted experimental setup and its corresponding required computational technique to process the data. This extends the above-mentioned potential advantages of GI to synchrotron XRF imaging. In addition, it enables new strategies to improve resilience against drifts at all scales and the study of previously inaccessible samples, such as liquids.

4D nanoimaging of early age cement hydration.

Despite a century of research, our understanding of cement dissolution and precipitation processes at early ages is very limited. This is due to the lack of methods that can image these processes with enough spatial resolution, contrast and field of view. Here, we adapt near-field ptychographic nanotomography to in situ visualise the hydration of commercial Portland cement in a record-thick capillary. At 19 h, porous C-S-H gel shell, thickness of 500 nm, covers every alite grain enclosing a water gap. The spatial dissolution rate of small alite grains in the acceleration period, ∼100 nm/h, is approximately four times faster than that of large alite grains in the deceleration stage, ∼25 nm/h. Etch-pit development has also been mapped out. This work is complemented by laboratory and synchrotron microtomographies, allowing to measure the particle size distributions with time. 4D nanoimaging will allow mechanistically study dissolution-precipitation processes including the roles of accelerators and superplasticizers.

Synchrotron X-ray imaging of the onset of ultrasonic horn cavitation.

High-power ultrasonic horns operating at low frequency are known to generate a cone-shaped cavitation bubble cloud beneath them. The exact physical processes resulting in the conical structure are still unclear mainly due to challenges associated with their visualization. Herein, we address the onset of the cavitation cloud by exploiting high-speed X-ray phase contrast imaging. It reveals that the cone formation is not immediate but results from a three-step phenomenology: (i) inception and oscillation of single bubbles, (ii) individual cloud formation under splitting or lens effects, and (iii) cloud merging leading to the formation of a bubble layer and, eventually, to the cone structure due to the radial pressure gradient on the horn tip.

Use of simulated experiments for material characterization of brittle materials subjected to high strain rate dynamic tension.

Rapid progress in ultra-high-speed imaging has allowed material properties to be studied at high strain rates by applying full-field measurements and inverse identification methods. Nevertheless, the sensitivity of these techniques still requires a better understanding, since various extrinsic factors present during an actual experiment make it difficult to separate different sources of errors that can significantly affect the quality of the identified results. This study presents a methodology using simulated experiments to investigate the accuracy of the so-called spalling technique (used to study tensile properties of concrete subjected to high strain rates) by numerically simulating the entire identification process. The experimental technique uses the virtual fields method and the grid method. The methodology consists of reproducing the recording process of an ultra-high-speed camera by generating sequences of synthetically deformed images of a sample surface, which are then analysed using the standard tools. The investigation of the uncertainty of the identified parameters, such as Young's modulus along with the stress-strain constitutive response, is addressed by introducing the most significant user-dependent parameters (i.e. acquisition speed, camera dynamic range, grid sampling, blurring), proving that the used technique can be an effective tool for error investigation.This article is part of the themed issue 'Experimental testing and modelling of brittle materials at high strain rates'.