Wissenschaftliche Artikel der BAM
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Determination of short carbon fiber orientation in zirconium diboride ceramic matrix composites
(2024)
In fiber-reinforced components, the fiber alignment and orientation have paramount influence on the thermomechanical properties of the resulting composite, for both short and continuous fiber. Here we present the case of an ultra-refractory matrix intended for extreme environment applications, ZrB2, reinforced with 20 vol% and 50 vol% short carbon fibers. In both cases, fibers tend to align perpendicular to the uniaxial pressure applied during shaping and sintering of a pellet, although the fiber tilt across the pellet thickness is difficult to determine. Moreover, for high volume fractions of reinforcement, the spatial distribution of the fibers is heterogeneous and tends to have domains of preferential orientations. We compare the information on the fiber distribution as collected by scanning electron microscopy images, X-ray computed tomography and synchrotron X-ray refraction radiography (SXRR). The three techniques prove to be complementary. Importantly, we demonstrate that SXRR yields the most statistically significant information due to the largest field of view, yet with a sensitivity down to the nanometer, and that can be successfully applied also to heavy matrix materials, such as zirconium boride.
Efficient density evolution during sintering of the as-printed component is vital to reach full densification and required properties of binder jet (BJT) components. However, due to the high porosity and brittle nature of the green compact, analysis of the microstructure development during sintering is very difficult, resulting in lack of understanding of the densification process. Density development from green state (57 ± 1.6 %) up to full density (99 ± 0.3 %) was characterized by high-resolution synchrotron X-Ray computed tomography (SXCT) on BJT 316L samples from ex-situ interrupted sintering tests. Periodicity of density fluctuations along the building direction was revealed for the first time and was related to the layer thickness of ~ 42 μm during printing that decreased down to ~ 33 μm during sintering. Sintering simulations, utilizing a continuum sintering model developed for BJT, allowed to replicate the density evolution during sintering with a mean error of 2 % and its fluctuation evolution from green (1.66 %) to sintered (0.56 %) state. Additionally, simulation of extreme particle size segregation (1 μm to 130 μm) suggested that non-optimized printing could lead to undesirable density fluctuation amplitude rapid increase (~10 %) during sintering. This might trigger the nucleation of defects (e.g., layer delamination, cracking, or excessive residual porosity) during the sintering process.
Simulation-Assisted Augmentation of Missing Wedge and Region-of-Interest Computed Tomography Data
(2024)
This study reports a strategy to use sophisticated, realistic X-ray Computed Tomography (CT) simulations to reduce Missing Wedge (MW) and Region-of-Interest (RoI) artifacts in FBP (Filtered Back-Projection) reconstructions. A 3D model of the object is used to simulate the projections that include the missing information inside the MW and outside the RoI. Such information augments the experimental projections, thereby drastically improving the reconstruction results. An X-ray CT dataset of a selected object is modified to mimic various degrees of RoI and MW problems. The results are evaluated in comparison to a standard FBP reconstruction of the complete dataset. In all cases, the reconstruction quality is significantly improved. Small inclusions present in the scanned object are better localized and quantified. The proposed method has the potential to improve the results of any CT reconstruction algorithm.
AbstractLithium‐ion cells connected in series are prone to an electrical safety risk called overdischarge. This paper presents a comprehensive investigation of the overdischarge phenomenon in lithium‐ion cells using operando nondestructive imaging. The study focuses on understanding the behavior of copper dissolution and deposition during overdischarge, which can lead to irreversible capacity loss and internal short‐circuits. By utilizing synchrotron X‐ray computed tomography (SXCT), the concentration of dissolved and deposited copper per surface area is quantified as a function of depth of discharge, confirming previous findings. The results also highlight for the first time a nonuniform distribution pattern for copper deposition on the cathode. This research provides insights for safer battery cell design.
It is shown that preconditioning of experimental X‐ray computed tomography (XCT) data is critical to achieve high‐precision segmentation scores. The challenging experimental XCT datasets and deep convolutional neural networks (DCNNs) are used that are trained with low‐resemblance synthetic XCT data. The material used is a 6‐phase Al–Si metal matrix composite‐reinforced with ceramic fibers and particles. To achieve generalization, in our past studies, specific data augmentation techniques were proposed for the synthetic XCT training data. In addition, two toolsets are devised: (1) special 3D DCNN architecture (3D Triple_UNet), slicing the experimental XCT data from multiple views (MultiView Forwarding), the i.S.Sy.Da.T.A. iterative segmentation algorithm, and (2) nonlocal means (NLM) conditioning (filtering) for the experimental XCT data. This results in good segmentation Dice scores across all phases compared to more standard approaches (i.e., standard UNet architecture, single view slicing, standard single training, and NLM conditioning). Herein, the NLM filter is replaced with the deep conditioning framework BAM SynthCOND introduced in a previous publication, which can be trained with synthetic XCT data. This leads to a significant segmentation precision increase for all phases. The proposed methods are potentially applicable to other materials and imaging techniques.
In the present study, in-situ observation of Hot Isostatic Pressure (HIP) procedure of laser powder bed fusion manufactured Ti-6Al-4V parts was performed to quantitatively estimate the densifcation rate of the material and the infuence of the defect initial size and shape on such rate. The observations were performed in-situ using the Ultrafast Tomography Paris-Edinburgh Cell and the combination of fast phase-contrast synchrotron X-ray tomography and energy dispersive difraction. With this strategy, we could quantify how the efectiveness of HIP depends on the characteristics of a defect. Smaller defects showed a higher densifcation rate, while the defect shape did not have signifcant efect on such rate.
The stress–strain behavior of ceramics, such as aluminum titanate, has certain features that are unusual for brittle materials—in particular, a substantial nonlinearity under uniaxial tension, and load–unload hysteresis caused by the sharp increase of the incremental stiffness at the beginning of unloading. These features are observed experimentally and are attributed to microcracking. Here we compare different degrees of stress–strain nonlinearity of aluminum titanate materials and quantitatively model them. We use advanced mechanical testing to observe the mechanical response at room and high temperature; electron microscopy, and X-ray refraction radiography to observe the microstructural changes. Experiments show that two types of microcracks can be distinguished: (i) microcracks induced by cooling from the sintering temperature (due to heterogeneity and anisotropy of thermal expansion), with typical sizes of the order of grain size, and (ii) much larger microcracks generated by the mechanical loading. The two microcrack types produce different effects on the stress–strain curves. Such microcracks and the features of the stress–strain behavior depend on the density of the cooling-induced microcracks and on the distribution of grain sizes. They are modeled analytically and numerically.
The peak broadening in neutron diffraction experiments on tensile specimens of pure Al (99.8%) and an Al-Mg alloy pre-deformed at different creep strains is analysed. These results are combined with the kernel angular misorientation of electron backscatter diffraction data from the creep-deformed microstructures. It is found that differently oriented grains possess different microstrains. These microstrains vary with creep strain in pure Al, but not in the Al-Mg alloy. It is proposed that this behaviour can explain the power-law breakdown in pure Al and the large creep strain observed in Al-Mg. The present findings further corroborate a description of the creep-induced dislocation structure as a fractal, predicated on previous work.
The damage mechanisms of metallic components produced by process laser powder bed fusion differ significantly from those typically observed in conventionally manufactured variants of the same alloy. This is due to the unique microstructures of additively manufactured materials. Herein, the focus is on the study of the evolution of creep damage in stainless steel 316L specimens produced by laser powder bed fusion. X-ray computed tomography is used to unravel the influence of the process-specific microstructure from the influence of the initial void distribution on creep damage mechanisms. The void distribution of two specimens tested at 600 °C and 650 °C is analyzed before a creep test, after an interruption, and after fracture. The results indicate that the formation of damage is not connected to the initial void distribution. Instead, damage accumulation at grain boundaries resulting from intergranular cracking is observed.
The hard X-ray beamline BAMline at BESSY II (Berlin, Germany) has now been in service for 20 years. Several improvements have been implemented in this time, and this review provides an overview of the imaging methods available at the BAMline. Besides classic full-field synchrotron X-ray computed tomography (SXCT), also absorption edge CT, synchrotron X-ray refraction radiography (SXRR), and synchrotron X-ray refraction tomography (SXRCT) are used for imaging. Moreover, virtually any of those techniques are currently coupled in situ or operando with ancillary equipment such as load rigs, furnaces, or potentiostats. Each of the available techniques is explained and both the current and the potential usage are described with corresponding examples. The potential use is manifold, the examples cover organic materials, composite materials, energy-related materials, biological samples, and materials related to additive manufacturing. The article includes published examples as well as some unpublished applications.