High-speed Synchrotron X-ray Imaging Research Articles

Direct observation of crack formation mechanisms with operando Laser Powder Bed Fusion X-ray imaging

Laser powder bed fusion ( L -PBF) is a versatile additive manufacturing process that can print geometrically complex metal parts for a variety of applications. However, poor control of defect formation during processing hampers its widespread industrial adoption. Many materials suffer from a high crack susceptibility during L -PBF, which results in degraded mechanical properties, and is an obstacle to the certification of critical parts. In order to unveil the mechanisms of crack formation in a prone-to-cracking nickel-based superalloy, we employ high-speed synchrotron X-ray imaging in combination with a miniaturized L -PBF set-up that reproduces real processing conditions. This unique set-up provides operando imaging of crack formation during L -PBF. Complementary post-mortem inspection of crack morphology and thermal simulations supported by operando X-ray diffraction-based measurements of the temperature evolution allow to identify the cracking mechanism and to differentiate solidification cracking from liquation.

In situ high-speed synchrotron X-ray imaging of laser-based directed energy deposition of the alloying process with dissimilar powders

Laser-based directed energy deposition (DED) additive manufacturing (AM) of the alloying process is performed using mixtures of Mo, Nb, Ti, and V powders and directly observed through in situ high-speed synchrotron X-ray imaging. The investigation on the integration of dissimilar powders into a single melt pool will narrow the gaps between the applied research and the fundamental understanding of the impact of different elemental powders on melt pool properties and defect production in the alloying formation via DED AM. The different traveling trajectories of four types of powders are revealed, such as the trajectories of most Mo powders on the top surface of the melt pool and the trajectories of Nb powders along with the melt flow. The melting modes, melting times, and the size changes of these four-element powders during the alloying process are obtained. Ti powders melt the fastest among these four powders. Ti and V powders melt near the site where they are delivered to the melt pool, while Mo and Nb powders melt when traveling with melt flow. The dynamics and velocities of melt flow in different sections of the melt pool are revealed, and the velocities and fluctuations near the area of the laser beam with the range from 0.134 m/s to 0.849 m/s are the largest in melt pool flow. The melt flow will benefit the uniform element distributions in the fabricated alloy. This study will provide a fundamental understanding of alloying formation via DED AM processes.

Characterization of keyhole dynamics in laser welding of copper by means of high-speed synchrotron X-ray imaging

Laser welding of copper is of great importance for industrial applications, e.g., for manufacturing of electrical components such as hairpins. Solid state lasers are widely used due to the high power and beam brilliance, but the implementation can be challenging in terms of process instabilities and resulting weld defects, i.e., spatter and pore formation. In order to understand the formation thus avoid these defects, the development of the understanding of the keyhole and its interaction with the surrounding melt pool is required. In this paper, high-speed synchrotron X-ray imaging (frame rate: 20,000 Hz) demonstrated its capability to study the keyhole geometry to quantify and describe the dynamic behavior inside the workpiece. Thus, novel insights into fundamental processes are provided and a new methodic approach was introduced to describe the time-dependent behavior of the keyhole and its interaction with the melt pool during laser beam deep welding of copper (Cu-ETP/CW004A).

In situ X-ray and thermal imaging of refractory high entropy alloying during laser directed deposition

MoNbTiV high-entropy alloy was in situ alloyed with laser power-blown directed energy deposition additive manufacturing from a mixture of four elemental powders of Mo, Nb, Ti, and V. This study provides a fundamental understanding of the alloying process through in situ high-speed synchrotron X-ray imaging and infrared imaging. High-speed X-ray imaging was used to investigate the in situ alloying process through direct observation. The particle delivery velocities of four different elemental powders under the same processing conditions were studied to reveal the performance of the powders during the in situ alloying process. We found that the Ti and Nb powders showed the greatest and smallest averaged particle-delivery velocities among these four powders, respectively, and the particle delivery velocity would be affected by the particle characteristics, particle size, and density of powders. The velocities of the resulting melt pool flow were measured to show the melt flow dynamics in such a process. The residence time of each elemental powder was also obtained, and Mo powders showed the largest residence time followed by Nb, V, and Ti powders. The porosity induced by unmelted particles and entrapped gas occurred in the alloying process. The Mo powders resulted in the most unmelted particles, and the entrapped gas porosity was mainly induced by the keyhole fluctuation. With the assistance of an infrared camera, we reported the emissivity of the melt pool, the change of thermal properties, and melt pool morphology during alloying.

Influence of the laser cutting front geometry on the striation formation analysed with high-speed synchrotron X-ray imaging

The generation of low surface roughness of the cut edge during laser beam cutting is a challenge. The striation pattern, which determines the surface roughness, can be distinguished into regular and interrupted striations, the latter resulting in an increased surface roughness. In order to analyse their formation, the space- and time-resolved cutting front geometry and melt film thickness were captured during laser beam fusion cutting of aluminium sheets with a framerate of 1000 Hz by means of high-speed synchrotron X-ray imaging. The comparison of the contours of the cutting fronts for a cut result with regular und interrupted striations shows that the contour fluctuates significantly more in case of interrupted striations. This leads to a strong fluctuation of the local angle of incidence. In addition, the average angle of incidence decreases, which results in an increase of the average absorbed irradiance. Both phenomena, local increase of absorbed irradiance and its dynamic fluctuation, result in a local increase of the melt film thickness at the cutting front which is responsible for the formation of the interrupted striations.

In-Situ Characterization of Pore Formation Dynamics in Pulsed Wave Laser Powder Bed Fusion.

Laser powder bed fusion (LPBF) is an additive manufacturing technology with the capability of printing complex metal parts directly from digital models. Between two available emission modes employed in LPBF printing systems, pulsed wave (PW) emission provides more control over the heat input compared to continuous wave (CW) emission, which is highly beneficial for printing parts with intricate features. However, parts printed with pulsed wave LPBF (PW-LPBF) commonly contain pores, which degrade their mechanical properties. In this study, we reveal pore formation mechanisms during PW-LPBF in real time by using an in-situ high-speed synchrotron x-ray imaging technique. We found that vapor depression collapse proceeds when the laser irradiation stops within one pulse, resulting in occasional pore formation during PW-LPBF. We also revealed that the melt ejection and rapid melt pool solidification during pulsed-wave laser melting resulted in cavity formation and subsequent formation of a pore pattern in the melted track. The pore formation dynamics revealed here may provide guidance on developing pore elimination approaches.

Synchrotron X-ray Analysis of the Influence of the Magnesium Content on the Absorptance during Full-Penetration Laser Welding of Aluminum

Full-penetration laser beam welding is characterized by a weld seam whose depth equals the material thickness. It is associated with a stable capillary and is therefore widely used for welding of sheet metal components. The realization of lightweight concepts in car body production requires the application of high-strength aluminum alloys that contain magnesium as an alloying element, which significantly influences the evaporation temperature and pressure. This change of the evaporation processes influences the geometry of the capillary and therefore its absorptance. In order to quantify the influence of magnesium on the capillary, their geometries were captured by means of high-speed synchrotron X-ray imaging during the welding process of the aluminum alloys AA1050A (Al99.5), AA5754 (AlMg3) and AA6016 (AlSi1.2Mg0.4). The 3D-geometries of the capillaries were reconstructed from the intensity distribution in the recorded X-ray images and their absorptance of the incident laser beam was determined by the analysis of the reconstructed 3D-geometry with a raytracing algorithm. The results presented in this paper capture for the first time the influence of the magnesium content in high-strength aluminum alloys on the aspect ratio of the capillary, which explains the reduced absorptance in case of full-penetration laser beam welding of aluminum alloys with a high content of volatile elements. In order to improve the absorptance in full-penetration welding, these findings provide the information required for the deduction of new optimization approaches.

The causal relationship between melt pool geometry and energy absorption measured in real time during laser-based manufacturing

During laser powder bed fusion additive manufacturing, laser power absorption is governed by a protean pool of molten metal that can present as a highly reflective surface, a deeply absorbing cavity, or some amalgamation thereof. These melt pool dynamics have been linked to defect creation, porosity, and surface finish quality. Although these are therefore critical for determining final part quality, their instantaneous influence on laser absorption have only been explored through simulation. To date, direct real-time observations have been elusive due to the locally extreme environment. In this work, we focus a laser on Ti-6Al-4V powder and bare plate while quantifying the time-dependent, absolute energy absorption by monitoring omnidirectional backscattered laser intensity. We also simultaneously record the projective melt pool geometries with high-speed synchrotron x-ray imaging. We find that laser absorption strongly reflects the stability of the vapor depression over a wide range of applied laser powers, oxygen content in the processing atmosphere, and with the presence of powder. During laser scanning of a powder bed surface, we find a significant absorption reduction after 400 µs due to a dramatic change in the vapor depression aspect ratio – an event known to create porosity. As several industrial scan strategies necessitate thousands of these events during a build, their identification and control is of significant practical importance. Lastly, a normalized enthalpy model is demonstrated to be effective in quantifying the relationship between the laser absorption and cavity depth, even under transient conditions. In addition to providing vital quantitative data for simulation calibration, the correlation of melt pool geometry with laser absorption during realistic processing conditions suggests the use of a total backscattered light detection system for real-time process control.

Synchrotron X-ray imaging and ultrafast tomography in situ study of the fragmentation and growth dynamics of dendritic microstructures in solidification under ultrasound

High speed synchrotron X-ray imaging and ultrafast tomography were used to study in situ and in real time the fragmentation and growth dynamics of dendritic microstructures of an Al-15%Cu alloy in solidification under ultrasound. An ultrasound of 30 kHz with vibration amplitude of 29 µm was applied into the alloy melt and produced a strong swirling acoustic flow of ~0.3 m/s. Efficient dendrite fragmentation occurred due to the acoustic flow and the dominant mechanism is the thermal perturbation remelting plus mechanical fracture and separation effect. Acoustic flow fatigue impact and phase collision effects were found to play a minor role in causing dendrite fragmentation. Just 10 s of ultrasound application at the early stage of solidification produced ~100% more dendrite fragments compared to the case without ultrasound, resulting in 20~25% reduction in the average grain size in the solidified samples. Furthermore, the dendrite morphology and tip growth velocity were mainly affected by the initial dendrite fragment number density and their distribution. The systematic and real-time datasets obtained in near operando conditions provided valuable 4D information for validation of numerical models and assistance in developing optimisation strategy for ultrasound melt processing in industry.

Nonlinear elasticity and damping govern ultrafast dynamics in click beetles

Many small animals use springs and latches to overcome the mechanical power output limitations of their muscles. Click beetles use springs and latches to bend their bodies at the thoracic hinge and then unbend extremely quickly, resulting in a clicking motion. When unconstrained, this quick clicking motion results in a jump. While the jumping motion has been studied in depth, the physical mechanisms enabling fast unbending have not. Here, we first identify and quantify the phases of the clicking motion: latching, loading, and energy release. We detail the motion kinematics and investigate the governing dynamics (forces) of the energy release. We use high-speed synchrotron X-ray imaging to observe and analyze the motion of the hinge's internal structures of four Elater abruptus specimens. We show evidence that soft cuticle in the hinge contributes to the spring mechanism through rapid recoil. Using spectral analysis and nonlinear system identification, we determine the equation of motion and model the beetle as a nonlinear single-degree-of-freedom oscillator. Quadratic damping and snap-through buckling are identified to be the dominant damping and elastic forces, respectively, driving the angular position during the energy release phase. The methods used in this study provide experimental and analytical guidelines for the analysis of extreme motion, starting from motion observation to identifying the forces causing the movement. The tools demonstrated here can be applied to other organisms to enhance our understanding of the energy storage and release strategies small animals use to achieve extreme accelerations repeatedly.

High-speed synchrotron X-ray imaging of directed energy deposition of titanium: effects of processing parameters on the formation of entrapped-gas pores

Laser based directed energy deposition (DED) is a competitive method for repairing and remanufacturing metallic parts used in numerous industries including aerospace and biomedical. However, the numerous dynamic phenomena associated with the DED process often result in defects such as entrapped-gas pores, lack of fusion, and undesirable anisotropic properties. The entrapped-gas pore, being one of the most common issues, not only influences melt-pool dynamics but also reduces the fabrication quality and mechanical properties of parts fabricated by the DED process. To reduce and further understand this issue, the real-time observation of the pore formation process needs to be studied first. To directly observe the phenomena in the melt pool, high-speed techniques are needed because rapid solidification leads to rapid pore formation and movement. In-situ high-speed X-ray has been proven to be an effective method in investigating the melt pool dynamics and pore formation mechanisms in the laser powder bed fusion process, in which the fabrication process is quite different from that in DED. Here, the high-speed X-ray method is extended to study the formation of entrapped-gas pores. The real-time formation and quantitative analysis of pores under each set of processing parameters (particle velocity, laser power, and spot welding dwelling time of stationary laser) in the DED process are investigated. We found that the DED with a higher particle velocity (3.19 m/s) produced a smaller average pore size of 27.8 µm and a lower pore area fraction of 0.52%. The DED under lower laser power (156 W) generated a smaller average pore size of 20.3 µm and a lower pore area fraction of 1.94%. The shorter dwelling time (10 ms) benefited the decrease of both average pore size and pore area fraction.

Simultaneous high-speed ultrasound and synchrotron x-ray imaging for monitoring melt pool dynamics in metallic additive manufacturing

Fundamental to metallic additive manufacturing (AM) is the laser-powder-substrate interaction that leads to localized melting of metallic powder to a previously solidified substrate. The formation of the melt pool and the subsequent solidification dictate the resultant microstructures and properties of the processed materials, which then influence both part quality and performance. Open ended questions involving the optimization of process parameters for defect free and high performing parts remain at the heart of AM science. Further understanding of melt pool and solidification behavior is required to help answer these questions. In this presentation, 25 MHz ultrasonic shear waves are used to probe dynamic melt pool behavior in Al6061 by observing the scattering from the solid/liquid and liquid/gas boundaries. High-speed synchrotron x-ray imaging was employed simultaneously with the ultrasonic measurement for validation. Melt pool features observed in the x-ray images were then associated with features in the synced ultrasound measurement. Specifically, the scattered response tracked with the depth of the melt pool. Finite element models depicting wave-scattering were also used to predict wave scattering and help interpret the ultrasonic response. These preliminary results provide support for ultrasonic scattering as a promising method to evaluate melt pool behavior in metallic additive manufacturing processes.

In situ radiographic and ex situ tomographic analysis of pore interactions during multilayer builds in laser powder bed fusion

Porosity and high surface roughness can be detrimental to the mechanical performance of laser powder bed fusion (LPBF) additive manufactured components, potentially resulting in reduced component life. However, the link between powder layer thickness on pore formation and surface undulations in the LPBF parts remains unclear. In this paper, the influence of processing parameters on Ti-6Al-4 V additive manufactured thin-wall components are investigated for multilayer builds, using a custom-built process replicator and in situ high-speed synchrotron X-ray imaging. In addition to the formation of initial keyhole pores, the results reveal three pore phenomena in multilayer builds resulting from keyhole melting: (i) healing of the previous layers' pores via liquid filling during remelting; (ii) insufficient laser penetration depth to remelt and heal pores; and (iii) pores formed by keyholing which merge with existing pores, increasing the pore size. The results also show that the variation of powder layer thickness influences which pore formation mechanisms take place in multilayer builds. High-resolution microcomputed tomography images reveal that clusters of pores form at the ends of tracks, and variations in the layer thickness and melt flow cause irregular remelting and track height undulations. Extreme variations in height were found to lead to lack of fusion pores in the trough regions. It is hypothesised that the end of track pores were augmented by soluble gas which is partitioned into the melt pool and swept to track ends, supersaturating during end of track solidification and diffusing into pores increasing their size.

Revealing transient powder-gas interaction in laser powder bed fusion process through multi-physics modeling and high-speed synchrotron x-ray imaging

Laser powder bed fusion (LPBF) is an emerging metal additive manufacturing process. The gas-driven powder motions in laser powder bed fusion have significant influence on the build quality. However, the transient powder-gas interaction has not been well understood due to the challenges in quantitative experiment measurements. In this work, the powder-gas interaction for a single pulse laser illuminating on the powder bed is studied. We establish a multi-physics model to simulate the complex liquid/gas flow as well as the gas-driven powder motions, which is substantiated by high-speed synchrotron x-ray imaging. We identify and quantify four characteristic modes of powder-gas interaction in LPBF. The motion of a powder is controlled by one or multiple interaction modes collectively. As revealed by simulations and confirmed by experiments, powders can merge into the molten pool from its rim, be ejected at different divergence angles (powder spattering), or dive into the molten pool to cause significant molten pool fluctuation. Our results provide insights toward the driving forces controlling the dynamic powder behavior, which pave the way for reducing structure defects during the build process.

High-speed synchrotron X-ray imaging of glass foaming and thermal conductivity simulation

Glass foams are attractive thermal insulation materials, thus, the thermal conductivity (λ) is crucial for their insulating performance. Understanding the foaming process is critical for process optimization. Here, we applied high-speed synchrotron X-ray tomography to investigate the change in pore structure during the foaming process, quantifying the foam structures and porosity dynamically. The results can provide guidance for the manufacturing of glass foams. The 3D pore structures were also used to computationally determine λ of glass foams using image-based modelling. We then used the simulated λ to develop a new analytical model to predict the porosity dependence of λ. The λ values of the glass foams when the porosity is within 40% to 95% predicted by the new model are in excellent agreement with the experimental data collected from the literature, with an average error of only 0.7%, which performs better than previously proposed models.

Investigation of dynamic fracture behavior of additively manufactured Al-10Si-Mg using high-speed synchrotron X-ray imaging

The dynamic tensile properties of additively manufactured (AM) and cast Al-10Si-Mg alloy were investigated using high-speed synchrotron X-ray imaging coupled with a modified Kolsky bar apparatus. A controlled tensile loading (strain rate ≈ 750 s−1) was applied using the Kolsky bar apparatus and the deformation and fracture behavior were recorded using the high-speed X-ray imaging setup. The synchrotron X-ray computed tomography (CT) and high-speed imaging results worked together to identify the location of the critical flaw and to capture the dynamics of crack propagation. In all experiments, the critical flaw was located on the surface of each specimen. The AM specimens showed significantly higher crack propagation speed, yield strength, ultimate tensile strength, strain hardening coefficient, and yet lower ductility compared to the cast specimens under dynamic tension. Although the strength values were higher for the AM specimens, the critical mode I stress intensity factors were comparable for both specimens. The microstructures of the samples were characterized by CT and scanning electron microcopy. The correlation between the dynamic fracture behavior of the samples and the microstructure of the samples is analyzed and discussed.

In situ Characterization of Laser Powder Bed Fusion Using High-Speed Synchrotron X-ray Imaging Technique

<i>In situ</i> Characterization of Laser Powder Bed Fusion Using High-Speed Synchrotron X-ray Imaging Technique

High-speed X-ray visualization of dynamic crack initiation and propagation in bone

The initiation and propagation of physiological cracks in porcine cortical and cancellous bone under high rate loading were visualized using high-speed synchrotron X-ray phase-contrast imaging (PCI) to characterize their fracture behaviors under dynamic loading conditions. A modified Kolsky compression bar was used to apply dynamic three-point flexural loadings on notched specimens and images of the fracture processes were recorded using a synchronized high-speed synchrotron X-ray imaging set-up. Three-dimensional synchrotron X-ray tomography was conducted to examine the initial microstructure of the bone before high-rate experiments. The experimental results showed that the locations of fracture initiations were not significantly different between the two types of bone. However, the crack velocities in cortical bone were higher than in cancellous bone. Crack deflections at osteonal cement lines, a prime toughening mechanism in bone at low rates, were observed in the cortical bone under dynamic loading in this study. Fracture toughening mechanisms, such as uncracked ligament bridging and bridging in crack wake were also observed for the two types of bone. The results also revealed that the fracture toughness of cortical bone was higher than cancellous bone. The crack was deflected to some extent at osteon cement line in cortical bone instead of comparatively penetrating straight through the microstructures in cancellous bone. Statement of SignificanceFracture toughness is with great importance to study for crack risk prediction in bone. For those cracks in bone, most of them are associated with impact events, such as sport accidents. Consequently, we visualized, in real-time, the entire processes of dynamic fractures in notched cortical bone and cancellous bone specimens using synchrotron X-ray phase contrast imaging. The onset location of crack initiation was found independent on the bone type. We also found that, although the extent was diminished, crack deflections at osteon cement lines, a major toughening mechanism in transversely orientated cortical bone at quasi-static rate, were still played a role in resisting cracking in dynamically loaded specimen. These finding help researchers to understand the dynamic fracture behaviors in bone.

Real time observation of binder jetting printing process using high-speed X-ray imaging

A high-speed synchrotron X-ray imaging technique was used to investigate the binder jetting additive manufacturing (AM) process. A commercial binder jetting printer with droplet-on-demand ink-jet print-head was used to print single lines on powder beds. The printing process was recorded in real time using high-speed X-ray imaging. The ink-jet droplets showed distinct elongated shape with spherical head, long tail, and three to five trailing satellite droplets. Significant drift was observed between the impact points of main droplet and satellite droplets. The impact of the droplet on the powder bed caused movement and ejection of the powder particles. The depth of disturbance in the powder bed from movement and ejection was defined as interaction depth, which is found to be dependent on the size, shape, and material of the powder particles. For smaller powder particles (diameter less than 10 μm), three consecutive binder droplets were observed to coalesce to form large agglomerates. The observations reported here will facilitate the understanding of underlying physics that govern the binder jetting processes, which will then help in improving the quality of parts manufactured using this AM process.

Modelling and experiments to identify high-risk failure scenarios for testing the safety of lithium-ion cells

Intentionally inducing worst-case thermal runaway scenarios in Li-ion cells on-demand is a definitive way to test the efficacy of battery systems in safely mitigating the consequences of catastrophic failure. An internal short-circuiting (ISC) device is implanted into three 18650 cell designs: one standard, one with a bottom vent, and one with a thicker casing. Through an extensive study of 228 cells, the position at which thermal runaway initiates is shown to greatly affect the tendency of cells to rupture and incur side-wall breaches at specific locations. The risks associated with each failure mechanism and position of the ISC device are quantified using a custom calorimeter that can decouple the heat from ejected and non-ejected contents. Causes of high-risk failure mechanisms, such as bursting and side-wall breaches, are elucidated using high-speed synchrotron X-ray imaging at 2000 frames per second and image-based 3D thermal runaway computational models, which together are used to construct a comprehensive description of external risks based on internal structural and thermal phenomena.