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- Additive manufacturing (8)
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- Residual stress (4)
- X-ray refraction (4)
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- Aluminum alloys (2)
- Ceramics (2)
- Creep (2)
- EBSD analysis (2)
- Electron beam melting (2)
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- 8 Zerstörungsfreie Prüfung (44)
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- 2 Prozess- und Anlagensicherheit (2)
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- 5.1 Mikrostruktur Design und Degradation (2)
- 7 Bauwerkssicherheit (2)
We show how the combination of the spatial autocorrelation function and permeability calculations, applied to 3D X-ray computed tomography data, can yield quantitative information on the anisotropy of both meso-structure and fluid flow in Diesel Particulate Filter (DPF) materials, such as Cordierite and SiC. It was found that both the degree of anisotropy, and the orientation of the permeability and meso-structure are similar, but not identical. We confirm that the morphological anisotropy of cordierite materials is weak, and clearly influenced by the extrusion process that determines the main direction of anisotropy. Properties of the autocorrelation function are discussed and it is shown why estimating the characteristic length of real meso-structures (grain or ?pore? size) is not possible. Finally, we show that the autocorrelation function applied on grey-level images can give a good estimate of the degree of anisotropy even with limited resolution.
The ability to track electrode degradation, both spatially and temporally, is fundamental to understand performance loss during operation of lithium batteries. X-ray computed tomography can be used to follow structural and morphological changes in electrodes; however, the direct detection of electrochemical processes related to metallic lithium is difficult due to the low sensitivity to the element. In this work, 4-dimensional neutron computed tomography, which shows high contrast for lithium, is used to directly quantify the lithium diffusion process in spirally wound Li/SOCl2 primary cells. The neutron dataset enables the quantification of the lithium transport from the anode and the accumulation inside the SOCl2 cathode to be locally resolved. Complementarity between the collected neutron and X-ray computed tomographies is shown and by applying both methods in concert we have observed lithium diffusion blocking by the LiCl protection layer and identified all cell components which are difficult to distinguish using one of the methods alone.
To assess the clinical course of a sheep stifle joint model for osteochondral (OC) defects, medial femoral condyles (MFC) were exposed without patella luxation using medial parapatellar skin (3–4 cm) and deep incisions (2–3 cm). Two defects (7 mm diameter; 10 mm depth; OC punch) were left empty or refilled with osteochondral autologous transplantation cylinders (OATS) and explanted after six weeks. Incision-to-suture time, anesthesia time, and postoperative wound or impairment scores were compared to those in sham-operated animals. Implant performance was assessed by X-ray, micro-computed tomography, histology, and immunohistology (collagens 1, 2; aggrecan). There were no surgery-related infections or patellar luxations. Operation, anesthesia, and time to complete stand were short (0.5, 1.4, and 1.5 h, respectively). The wound trauma score was low (0.4 of maximally 4; day 7). Empty-defect and OATS animals reached an impairment score of 0 significantly later than sham animals (7.4 and 4.0 days, respectively, versus 1.5 days). Empty defects showed incomplete healing and dedifferentiation/heterotopic differentiation; OATS-filled defects displayed advanced bone healing with remaining cartilage gaps and orthotopic expression of bone and cartilage markers. Minimally-invasive, medial parapatellar surgery of OC defects on the sheep MFC allows rapid and low-trauma recovery and appears well-suited for implant testing.
The relationship between residual stresses and microstructure associated with a laser powder bed fusion (LPBF) IN718 alloy has been investigated on specimens produced with three different scanning strategies (unidirectional Y-scan, 90° XY-scan, and 67° Rot-scan). Synchrotron X-ray energy-dispersive diffraction (EDXRD) combined with optical profilometry was used to study residual stress (RS) distribution and distortion upon removal of the specimens from the baseplate. The microstructural characterization of both the bulk and the nearsurface regions was conducted using scanning electron microscopy (SEM) and electron backscatter diffraction (EBSD). On the top surfaces of the specimens, the highest RS values are observed in the Y-scan specimen and the lowest in the Rot-scan specimen, while the tendency is inversed on the side lateral surfaces. A considerable amount of RS remains in the specimens after their removal from the baseplate, especially in the Y- and Z-direction (short specimen Dimension and building direction (BD), respectively). The distortion measured on the top surface following baseplate thinning and subsequent removal is mainly attributed to the amount of RS released in the build direction. Importantly, it is observed that the additive manufacturing microstructures challenge the use of classic theoretical models for the calculation of diffraction elastic constants (DEC) required for diffraction-based RS analysis. It is found that when the Reuß model is used for the calculation of RS for different crystal planes, as opposed to the conventionally used Kröner model, the results exhibit lower scatter. This is discussed in context of experimental measurements of DEC available in the literature for conventional and additively manufactured Ni-base alloys.
The understanding of dynamic processes in Li-metal batteries is an important consideration to enable the full capacity of cells to be utilised. These processes, however, are generally not directly observable using X-ray techniques due to the low attenuation of Li; and are challenging to visualise using neutron imaging due to the low temporal resolution of the technique. In this work, complementary X-ray and neutron imaging are combined to track the dynamics of Li within a primary Li/SOCl2 cell. The temporal challenges posed by neutron imaging are overcome using the golden ratio imaging method which enables the identification of Li diffusion in operando. This combination of techniques has enabled an improved understanding of the processes which limit rate performance in Li/SOCl2 cells and may be applied beyond this chemistry to other Li-metal cells.
This article highlights Peter Paufler’s academic genealogy on the occasion of his 80th birthday. We describe the academic background since 1776, which covers 11 generations of scientists: Ritter, Ørsted, Hansteen, Keilhau, Kjerulf, Brøgger, Goldschmidt, Schulze, Paufler, Meyer, and Leisegang. The biographies of these scientists are described in spotlight character and references to scientists such as Dehlinger, Ewald, Glocker, Röntgen, Vegard, Weiss, and Werner are given. A path is drawn that begins in the Romanticism with electrochemistry and the invention of what is probably the first accumulator. It leads through the industrialization and the modern geology, mineralogy, and crystallography to crystal chemistry, metal and crystal physics and eventually returns to electrochemistry and the aluminum-ion accumulator in the era of the energy transition. The academic genealogy exhibits one path of how crystallography develops and specializes over three centuries and how it contributes to the understanding of the genesis of the Earth and the Universe, the exploration of raw materials, and the development of modern materials and products during the industrialization and for the energy transition today. It is particularly characterized by the fields of physics and magnetism, X-ray analysis, and rare earth compounds and has strong links to the scientific landscape of Germany (Freiberg) and Scandinavia, especially Norway (Oslo), as well as to Russia (Moscow, Samara, St. Petersburg). The article aims at contributing to the history of science, especially to the development of crystallography, which is the essential part of the structural science proposed by Peter Paufler.
Modern air-liners and wind turbine rotor blades are made up primarily of fiber reinforced plastics. Failure of these materials heavily impairs the serviceability and the operational safety. Consequently, knowledge of the failure behavior under static and cyclic loads is of great interest to estimate the operational strength and to compare the performance of different materials. Ideally, the damage evolution under operational load is determined with in situ non-destructive testing techniques. Here, we report in-situ synchrotron X-ray imaging of tensile stress induced cracks in carbon fiber reinforced plastics due to inter-fiber failure. An inhouse designed compact tensile testing machine with a load range up to 15 kN was integrated into the beamline. Since conventional radiographs do not reveal sufficient contrast to distinguish cracks due to inter-fiber failure and micro cracking from fiber bundles, the Diffraction Enhanced Imaging (DEI) technique is applied in order to separate primary and scattered (refracted) radiation by means of an analyzer crystal. This technique allows fast measurements over large fields-of-view and is ideal for in-situ investigations. Imaging and the tensile test are run at the highest possible frame rate (0.7 s-1 ) and the lowest possible strain rate (5.5∙10-4 s -1 ). For 0°/90° non-crimp fabrics, the first inter-fiber cracks occur at 380 MPa (strain 0.8 %). Prior to failure at about 760 MPa (strain 2.0 %), we observe the evolution of nearly equidistant (1 mm distance) cracks running across the entire sample in the fully damaged state.
X-Ray computed tomography and traditional analysis of a capillary absorption test in cement pastes
(2020)
Water absorption testing has the attraction of being simple, relatively quick and use water as a fluid which is the key substance in the possible concrete deterioration. However, in spite of the advantages its application has remained empirical, except for the testing of resistance to frost, through the identification of the critical degree of saturation. Rilem TC-116 studied this test, among others, for the characterization of concrete resistance against transport through the concrete pore network. Results indicated a low discriminating ability of the absorbency for qualifying concrete resistance and then, it seemed necessary to try to move forward by making the link between the absorption testing and the concrete pore microstructure. In the present work, thanks to the X-Ray computed tomography, it is described the evolution of the water front in three paste-specimen with different w/c ratios (different pore radius distributions). The observations allowed us to deduce that all the pores start to fill simultaneously, but the bigger ones fill quicker and rise less. The saturation degree is measured along the height of the sample, showing that each pore size has a different rate which becomes constant after the first hour. Washburn’s equation was applied to the progressive advance of the water front, resulting in a pore radius much smaller than the one expected.
The mechanisms controlling the fatigue response of an A357-T6 cast aluminium alloy under cyclic torsional loading are investigated. Surface crack monitoring coupled with Electron BackScattering Diffraction (EBSD) analysis is used to study crack initiation. Determination of S-N curve combined with interrupted in situ fatigue testing using synchrotron tomography allows the study of the propagation behaviour. It is observed that fractographic morphologies depend on the stress level. At intermediate-low stress levels ( τmax < 100 MPa), the grain structure controls the crack initiation and propagation periods. Cracks are usually nucleated in mode II from slip planes close to the specimen axis or perpendicular to it. Mode II crack growth dominates the early stages of crack propagation as mode III inward crack growth is rapidly decelerated. This behaviour leads to the formation of characteristic shallow surface cracks. Once the crack is long enough for the mode II driving force to be overtaken by mode III, propagation branches into ~45 ◦mode I.
The goal of the Special Issue “Brittle Materials in Mechanical Extremes” was to spark a discussion of the analogies and the differences between different brittle materials, such as, for instance, ceramics and concrete. Indeed, the contributions to the Issue spanned from construction materials (asphalt and concrete) to structural ceramics, reaching as far as ice. The data shown in the issue were obtained by advanced microstructural techniques (microscopy, 3D imaging, etc.) and linked to mechanical properties (and their changes as a function of aging, composition, etc.). The description of the mechanical behavior of brittle materials under operational loads, for instance, concrete and ceramics under very high temperatures, offered an unconventional viewpoint on the behavior of brittle materials. This is not at all exhaustive, but a way to pave the road for intriguing and enriching comparisons.
The present work offers an explanation on how the long-range interaction of dislocations influences their movement, and therefore the strain, during creep of metals. It is proposed that collective motion of dislocations can be described as a fractional Brownian motion. This explains the noisy appearance of the creep strain signal as a function of time. Such signal is split into a deterministic and a stochastic part. These terms can be related to two kinds of dislocation motions: individual and collective, respectively. The description is consistent with the fractal nature of strain-induced dislocation structures predicated in previous works. Moreover, it encompasses the evolution of the strain rate during all stages of creep, including the tertiary one. Creep data from Al99.8% and Al- 3.85%Mg tested at different temperatures and stresses are used to validate the proposed ideas: it is found that different creep stages present different diffusion characters, and therefore different dislocation motion character.
X-ray computed tomography has many applications in materials science and non-destructive testing. While the standard filtered back-projection reconstruction of the radiographic data sets is fast and simple, it typically fails in returning accurate results from missing or inconsistent projections. Among the alternative techniques that have been proposed to handle such data is the Direct Iterative REconstruction of Computed Tomography Trajectories (DIRECTT) algorithm. We describe a new approach to the algorithm, which significantly decreases the computational time, while achieving a better reconstruction quality than that of other established algorithms.
Rapid cooling rates and steep temperature gradients are characteristic of additively manufactured parts and important factors for the residual stress formation. This study examined the influence of heat accumulation on the distribution of residual stress in two prisms produced by Laser Powder Bed Fusion (LPBF) of austenitic stainless steel 316L. The layers of the prisms were exposed using two different border fill scan strategies: one scanned from the centre to the perimeter and the other from the perimeter to the centre. The goal was to reveal the effect of different heat inputs on samples featuring the same solidification shrinkage. Residual stress was characterised in one plane perpendicular to the building direction at the mid height using Neutron and Lab X-ray diffraction. Thermography data obtained during the build process were analysed in order to correlate the cooling rates and apparent surface temperatures with the residual stress results. Optical microscopy and micro computed tomography were used to correlate defect populations with the residual stress distribution. The two scanning strategies led to residual stress distributions that were typical for additively manufactured components: compressive stresses in the bulk and tensile stresses at the surface. However, due to the different heat accumulation, the maximum residual stress levels differed. We concluded that solidification shrinkage plays a major role in determining the shape of the residual stress distribution, while the temperature gradient mechanism appears to determine the magnitude of peak residual stresses.
In this work, which is part of a larger research program, a framework called “virtual data fusion“ was developed to provide an automated and consistent crack detection method that allows for the cross-comparison of results from large quantities of X-ray Computed Tomography (CT) data. A partial implementation of this method in a custom program was developed for use in research focused on crack quantification in Alkali-Silica Reaction (ASR)-sensitive concrete aggregates. During the CT image processing, a series of image analyses tailored for detecting specific, individual crack-like characteristics were completed. The results of these analyses were then “fused” in order to identify crack-like objects within the images with much higher accuracy than that yielded by any individual image analysis procedure. The results of this strategy demonstrated the success of the program in effectively identifying crack-like structures and quantifying characteristics, such as surface area and volume. The results demonstrated that the source of aggregate has a very significant impact on the amount of internal cracking, even when the mineralogical characteristics remain very similar. River gravels, for instance, were found to contain significantly higher levels of internal cracking than quarried stone aggregates of the same mineralogical type.
The effect of two types of scanning strategies on the grain structure and build-up of Residual Stress (RS) has been investigated in an as-built IN718 alloy produced by Laser Powder Bed Fusion (LPBF). The RS state has been investigated by X-ray diffraction techniques. The microstructural characterization was performed principally by Electron Backscatter Diffraction (EBSD), where the application of a post-measurement refinement technique enables small misorientations (< 2°) to be resolved. Kernel average misorientation (KAM) distributions indicate that preferably oriented columnar grains contain higher levels of misorientation, when compared to elongated grains with lower texture. The KAM distributions combined with X-ray diffraction stress maps infer that the increased misorientation is induced via plastic deformation driven by the thermal stresses, acting to self-relieve stress. The possibility of obtaining lower RS states in the build direction as a consequence of the influence of the microstructure should be considered when envisaging scanning strategies aimed at the mitigation of RS.
Due to the wide range of applications, the easy production and the large field of use, reinforced concrete (RC) is a widespread building material. This variety of applications is reflected in a wide range of physical material properties. Not only therefor it still is a technical challenge to provide all necessary test conditions for experimentally reproducing dynamic effects under impact loading of RC structures. In this paper we present investigations on the thicknesses of RC plates under low and medium high velocity impact loading by a flat-tipped impactor. The planar tomography setup at BAM is used to visualize the impact damage and to characterize the damage features such as cracks, scabbing and spalling. Further, the comparison of tomography results with those of an applied numeric simulation analysis is used to verify the numeric models for future damage prognosis under impact loading. Using the results of both, the tomographic as well as the FE analysis, different damage features were investigated and compared regarding their validity. Crack damage plays a leading part and the significance of summarized crack values as well as their distribution is analyzed. The total damage value but also the determined damage distribution both provide an input for describing damage as a function of the impactor velocity and plate thickness.
Herein, we present a detailed investigation of the electrochemically triggered formation and dissolution processes of α- and β-sulfur crystals on a monolithic carbon cathode using operando high-resolution synchrotron radiography (438 nm/pixel).
The combination of visual monitoring with the electrical current response during cyclic voltammetry provides valuable insights into the sulfur formation and dissolution mechanism. Our observations show that the crystal growth process is mainly dictated by a rapid equilibrium between long-chain polysulfides on one side and solid sulfur/short-chain polysulfides on the other side, which is consistent with previous studies in this field. The high temporal and spatial resolution of synchrotron imaging enables the observation of different regimes during the sulfur formation and dissolution process. The appearance of short-chain polysulfides after the first anodic CV peak initiates a rapid dissolution process of α-sulfur crystals on the cathode. The increase in the long-chain lithium polysulfide concentration at the cathode surface during charge results in an increased crystal growth rate, which in turn produces imperfections in α- and β-sulfur crystals. There are strong indications that these defects are fluid inclusions, which may trap dissolved polysulfides and therefore reduce the electrochemical cell capacity.
The contour scan strategies in laser powder bed fusion (LPBF) of Ti-6Al-4V were studied at the coupon level. These scan strategies determined the surface qualities and subsurface residual stresses. The correlations to these properties were identified for an optimization of the LPBF processing. The surface roughness and the residual stresses in build direction were linked: combining high laser power and high scan velocities with at least two contour lines substantially reduced the surface roughness, expressed by the arithmetic mean height, from values as high as 30 μm to 13 μm, while the residual stresses rose from ~340 to about 800 MPa. At this stress level, manufactured rocket fuel injector components evidenced macroscopic cracking. A scan strategy completing the contour region at 100 W and 1050 mm/s is recommended as a compromise between residual stresses (625 MPa) and surface quality (14.2 μm). The LPBF builds were monitored with an in-line twin-photodiode-based melt pool monitoring (MPM) system, which revealed a correlation between the intensity quotient I2/I1, the surface roughness, and the residual stresses. Thus, this MPM system can provide a predictive estimate of the surface quality of the samples and resulting residual stresses in the material generated during LPBF.
The creep strengthening mechanisms in (age-hardenable) aluminum alloys are analyzed on the basis of a new microstructural study of powder samples, an analysis of a comprehensive revision of creep data from the literature, and a new modeling approach. A strategy based on the strength difference (SD) method to separate the contributions of solid solution atoms and precipitates to creep strengthening is proposed. The new methodology considers the combination of the two contributions avoiding the need of a threshold stress term in the creep equation. The contribution of both precipitates and solid solution is taken into account by means of the analysis of the lattice parameter variation with aging time. For this study, powders of two commercial AA2xxx alloys have been analyzed using diffraction methods. The experimental results are modeled using Lubarda’s approach combined with the SD method.
The paper presents the results of a series of combined mechanical and in-situ morphological investigations on highstrength strain-hardening cement-based Composites (SHCC). Tension and compression experiments were performed in a CT scanner employing a dedicated mechanical testing rig. The in-situ microtomographic scans enabled correlating the measured specimen response with relevant microstructural features and fracture processes. The microstructural segmentation of SHCC was performed in the framework of Deep Learning and it targeted an accurate segmentation of pores, fibers and aggregates. Besides their accurate volumetric representation, these phases were quantified in terms of content, size and orientation. The fracture processes were monitored at different loading stages and Digital Volume Correlation (DVC) was employed to spatially map the strains and cracks in the specimens loaded in compression. The DVC analysis highlighted the effect of loading conditions, specimen geometry and material heterogeneity at the mesolevel on the strain distribution and fracture localization.
The paper is motivated by some inconsistencies and contradictions present in the literature on the calculation of the so-called diffraction elastic constants. In an attempt at unifying the views that the two communities of Materials Science and Mechanics of Materials have on the subject, we revisit and define the terminology used in the field. We also clarify the limitations of the commonly used approaches and Show that a unified methodology is also applicable to textured materials with a nearly arbitrary grain shape. We finally compare the predictions based on this methodology with experimental data obtained by in situ synchrotron radiation diffraction on additively manufactured Ti-6Al4V alloy. We show that (a) the transverse isotropy of the material yields good agreement between the best-fit isotropy approximation (equivalent to the classic Kröner’s model) and the experimental data and (b) the use of a general framework allows the calculation of all components of the tensor of diffraction elastic constants, which are not easily measurable by diffraction methods. This allows us to extend the
current state-of-the-art with a predictive tool.
Using SXRR to Probe the Nature of Discontinuities in SLM Additive Manufactured Inconel 718 Specimens
(2020)
The utilization of additive manufacturing (AM) to fabricate robust structural components relies on understanding the nature of internal anomalies or discontinuities, which can compromise the structural integrity. While some discontinuities in AM microstructures stem from similar mechanisms as observed in more traditional processes such as casting, others are unique to the AM process. Discontinuities in AM are challenging to detect, due to their submicron size and orientation dependency. Toward the goal of improving structural integrity, minimizing discontinuities in an AM build requires an understanding of the mechanisms of formation to mitigate their occurrence. This study utilizes various techniques to evaluate the shape, size, nature and distribution of discontinuities in AM Inconel 718, in a non-hot isostatic pressed (HIPed) as-built, non-HIPed and direct age, and HIPed with two step age samples. Non-destructive synchrotron radiation refraction and transmission radiography (SXRR) provides additional information beyond that obtained with destructive optical microscopy. SXRR was able to distinguish between voids, cracks and lack of melt in, due to its sensitivity to the orientation of the discontinuity.
Wire Arc Additive Manufacturing (WAAM) features high deposition rates and, thus, allows production of large components that are relevant for aerospace applications. However, a lot of aerospace parts are currently produced by forging or machining alone to ensure fast production and to obtain good mechanical properties; the use of these conventional process routes causes high tooling and material costs. A hybrid approach (a combination of forging and WAAM) allows making production more efficient. In this fashion, further structural or functional features can be built in any direction without using additional tools for every part. By using a combination of forging basic geometries with one tool set and adding the functional features by means of WAAM, the tool costs and material waste can be reduced compared to either completely forged or machined parts. One of the factors influencing the structural integrity of additively manufactured parts are (high) residual stresses, generated during the build process. In this study, the triaxial residual stress profiles in a hybrid WAAM part are reported, as determined by neutron diffraction. The analysis is complemented by microstructural investigations, showing a gradient of microstructure (shape and size of grains) along the part height. The highest residual stresses were found in the transition Zone (between WAAM and forged part). The total stress range showed to be lower than expected for WAAM components. This could be explained by the thermal history of the component.
Virtuelle CT
(2020)
Das Computerprogramm aRTist ist ein praktisches Simulationswerkzeug zur Erzeugung realistischer Radiographien virtueller Durchstrahlungsaufbauten. Mit Durchstrahlungssimulationen können Bauteile, repräsentiert durch STL-Geometrien, wie in einem Computertomografen gescannt werden. Dabei werden verschiedenste Parameter gezielt und exakt berücksichtigt.
Die Virtuelle Computertomografie bietet neue Möglichkeiten der Untersuchung von Parametereinflüssen. Neben der Möglichkeit, physikalische Effekte an- und abzuschalten, z.B. die Streustrahlung, können auch Scanbewegungen getestet werden, bevor diese technisch realisiert werden.
Das für die Forschung entwickelte Simulationsprogramm aRTist bietet mit seiner intuitiven grafischen Benutzeroberfläche vielfältige Anwendungsmöglichkeiten auch in Praxis und Entwicklung, beispielsweise zur Parameteroptimierung, für Machbarkeitsstudien oder zur Abschätzung der Unsicherheit dimensioneller Messungen.
The Stone Age site Riņņukalns, Latvia, is the only well-stratified shell midden in the Eastern Baltic. In this paper, we present new interdisciplinary results concerning its dating, stratigraphy, features, and finds to shed light on the daily life of a fisher population prior to the introduction of domesticated animals. The undisturbed part of the midden consists of alternating layers of unburnt mussel shell, burnt mussel shell and fish bone, containing artefacts, some mammal and bird bones, and human burials. Two of them, an adult man and a baby, are discovered recently and date to the calibration plateau between 3350 and 3100 cal BC, and to the later 4th millennium, respectively. Stable isotopes suggest a diet based heavily on freshwater fish, and this is supported not only by ten thousands of identified fish remains, but also by a fish bone concentration nearby the skull of the man, which is interpreted as remain of a grave gift (possible fish soup). Of special interest are the baby’s stable isotope values. It shows that the mother’s diet was atypical (perhaps because she was non-local), and/or that dietary stress during pregnancy increased fractionation between the mother’s diet and her bloodstream
Connecting Diffraction-Based Strain with Macroscopic Stresses in Laser Powder Bed Fused Ti-6Al-4V
(2020)
The laser powder bed fusion (LPBF) production process often results in large residual stress (RS) in the parts. Nondestructive techniques to determine RS are badly needed. However, a reliable quantification of macro-RS (i.e., stress at the component level) by means of diffraction-based techniques is still a great challenge, because the link between diffraction-based strain and macro-RS is not trivial. In this study, we experimentally determine (by means of in-situ synchrotron radiation diffraction) this link for LPBF Ti-6Al-4V. We compare our results with commonly used models to determine the so-called diffraction elastic constants (DECs). We show that LPBF materials possess different DECs than wrought alloys, simply because their microstructural and mechanical properties are different. We also show that the existing models can be used to calculate DECs only if high accuracy of the RS values is not required. If the peculiarities of the microstructure have to be taken into account (as is the case of additively manufactured materials), a radically new approach is desirable.
Explaining Deviatoric Residual Stresses in Aluminum Matrix Composites with Complex Microstructure
(2020)
The residual stresses in multiphase metal Matrix composites with both random planar-oriented short fibers and particles were studied by neutron diffraction and by a model based on the reformulation of classic Maxwell’s homogenization method. Contrary to common understanding and state-of-the-art models, we experimentally observed that randomly oriented phases possess non-hydrostatic residual stress. The recently developed modeling Approach allows calculating the residual stress in all phases of the composites. It rationalizes the presence of deviatoric stresses Accounting for the interaction of random oriented phases with fibers having preferential orientation.
An ultrasonic vibration post-treatment procedure was suggested for additively manufac-tured lattices. The aim of the present research was to investigate mechanical properties andthe differences in mechanical behavior and fracture modes of Ti6Al4V scaffolds treated withtraditional powder recovery system (PRS) and ultrasound vibration (USV). Scanning electronmicroscopy (SEM) was used to investigate the strut surface and the fracture surface mor-phology. X-ray computed tomography (CT) was employed to evaluate the inner structure,strut dimensions, pore size, as well as the surface morphology of additively manufacturedporous scaffolds. Uniaxial compression tests were conducted to obtain elastic modulus,compressive ultimate strength and yield stress. Finite element analysis was performedfor a body-centered cubic (BCC) element-based model and for CT-based reconstructiondata, as well as for a two-zone scaffold model to evaluate stress distribution during elasticdeformation. The scaffold with PRS post treatment displayed ductile behavior, while USVtreated scaffold displayed fragile behavior. Double barrel formation of PRS treated scaffoldwas observed during deformation. Finite element analysis for the CT-based reconstructionrevealed the strong impact of surface morphology on the stress distribution in comparisonwith BCC cell model because of partially molten metal particles on the surface of struts,which usually remain unstressed.
The material and damage behaviour of additively manufactured polyamide 12 under cyclic loading was characterized by cyclic tests and microstructure analysis by using microscopy, X-ray refraction, and computed tomography. The results were used to determine parameters for the viscoplastic material model by Chaboche and a damage model by Gurson-Tvergaard-Needleman. The temperature was monitored during the experiments and the self-heating effect was observed. By including this effect, a higher accuracy could be achieved with the results of mechanical experiments.
Ti-Al-Nb based intermetallic layers of sufficient quality and thickness were obtained by non-vacuum electron beam cladding on the surfaces of Ti workpieces. Optical microscopy and X-ray tomography did not reveal any dramatical defects in the structure of cladded layers. X-ray diffraction as well as scanning and transmission electron microscopy were applied to thoroughly investigate the structure and phase composition of coatings. It was found that non-equilibrium cooling conditions of coatings provided by fast removal of heat to untreated Ti substrate after the electron beam cladding was terminated induced the proceeding of metastable phase transformations. For example, γ-phase formation was suppressed in these coatings. In coatings with 8 and 20 at.% Nb (46 and 43% Al respectively) along with ordered with α2, formation of disordered solution of the alloying elements in α-Ti took place. In high-Nb alloys β(B2) phase has undergone the diffusionless transformation to ω’, which is the intermediate phase in β → ω and the coating with the maximum Nb content characterized by appearance of γ1 as a main phase. ω-phase had negative influence to hardness and wear resistance of coatings, however, generally this paremeter increased in 1.3–1.75 times compared to cp-Ti. The high temperature creep and oxidation properties decreased proportionally with increasing Nb and decreasing Al content in the cladded layers.
The mixture of ammonium nitrate (AN) prills and fuel oil (FO), usually referred to as ANFO, is extensively used in the mining industry as a bulk explosive. One of the major performance predictors of ANFO mixtures is the fuel oil retention, which is itself governed by the complex pore structure of the AN prills. In this study, we present how X-ray computed tomography (XCT), and the associated advanced data processing workflow, can be used to fully characterise the structure and morphology of AN prills. We show that structural parameters such as volume fraction of the different phases and morphological parameters such as specific surface area and shape factor can be reliably extracted from the XCT data, and that there is a good agreement with the measured oil retention values. Importantly, oil retention measurements (qualifying the efficiency of ANFO as explosives) correlate well with the specific surface area determined by XCT. XCT can therefore be employed non-destructively; it can accurately evaluate and characterise porosity in ammonium nitrate prills, and even predict their efficiency.
Porosity in additively manufactured materials, such as laser powder bed fusion Ti-Al6-V4, can play an important role in their mechanical performance. Not only the total porosity but also the shape/morphology of the individual pores need to be considered. Therefore, it is necessary to determine the distributions of different defect types (especially fusing defects and keyhole pores) and their dependence on process parameters. We show that synchrotron X-ray refraction radiography allows analysis of large samples (up to several millimeters) without compromising the detectability of submicrometer defects. Correspondingly, a classification tool is introduced that is able to quantitatively distinguish defects such as keyhole pores and binding defects with a confidence level of 94 %, even when the shape cannot be discerned because of limited spatial resolution.
This study reports the results of the preliminary assessment to fabricate Ti-10at% Nb alloy by electron beam melting (EBM®) from a blend of elemental Nb and Ti powders. The microstructure of the EBM-manufactured Ti-10at% Nb alloys is sensitive to the following factors: different sintering properties of Nb and Ti powders, powder particle properties, material viscosities at varying melt pool temperatures, β-stabilizer element content and the EBM® process parameters. Three phases were observed in as-manufactured Ti-10at% Nb alloy: μm-size Nb phase, a Nb-rich β-solid solution surrounding Nb phase, lamellar structured α-phase and β-solid solution with different distribution and volume fraction. Thus, the combination of powder particle characteristics, very short time material spends in molten condition and sluggish kinetics of mixing and diffusional process in Ti-Nb alloy results in heterogeneous microstructures depending on the local Nb content in the powder blend and the EBM® process conditions.
We show that the equation proposed by Takeuchi and Argon to explain the creep behavior of Al–Mg solid solution can be used to describe also the creep behavior of pure aluminum. In this frame, it is possible to avoid the use of the classic pre-exponential fitting parameter in the power law equation to predict the minimum creep strain rate. The effect of the fractal arrangement of dislocations, developed at the mesoscale, must be considered to fully explain the experimental data. These ideas allow improving the recently introduced SSTC model, fully describing the primary and secondary creep regimes of aluminum alloys without the need for fitting. Creep data from commercially pure Al99.8% and Al–Mg alloys tested at different temperatures and stresses are used to validate the proposed ideas.
The quantitative analysis of microstructural features is a key to understanding the micromechanical behavior of metal matrix composites (MMCs), which is a premise for their use in practice. Herein, a 3D microstructural characterization of a five-phase MMC is performed by synchrotron X-ray computed tomography (SXCT). A workflow for advanced deep learning-based segmentation of all individual phases in SXCT data is shown using a fully convolutional neural network with U-net architecture. High segmentation accuracy is achieved with a small amount of training data. This enables extracting unprecedently precise microstructural parameters (e.g., volume fractions and particle shapes) to be input, e.g., in micromechanical models.
The creep strengthening mechanisms in (age-hardenable) aluminum alloys are analyzed on the basis of a new microstructural study of powder samples, an analysis of a comprehensive revision of creep data from the literature, and a new modeling approach. A strategy based on the strength difference (SD) method to separate the contributions of solid solution atoms and precipitates to creep strengthening is proposed. The new methodology considers the combination of the two contributions avoiding the need of a threshold stress term in the creep equation. The contribution of both precipitates and solid solution is taken into account by means of the analysis of the lattice parameter variation with aging time. For this study, powders of two commercial AA2xxx alloys have been analyzed using diffraction methods. The experimental results are modeled using Lubarda's approach combined with the SD method.
Ammonium nitrate (AN) prills are commonly used as an ingredient in industrial explosives and in fertilisers. Conventional techniques (such as BET or mercury intrusion porosimetry) can measure the open porosity and specific surface area of AN prill, but the closed porosity is not obtainable. This work was focused on evaluating X-ray computed tomography (XCT) as a non-destructive technique for the assessment of porosity in AN prills. An advanced data processing workflow was developed so that the segmentation and quantification of the CT data could be performed on the entire 3D volume, yet allowing the measurements (e.g.; volume, area, shape factor…) to be extracted for each individual phase (prill, open porosity, closed porosity) of each individual prill, in order to obtain statistically relevant data. Clear morphological and structural differences were seen and quantified between fertiliser and explosive products. Overall, CT can provide a very wide range of parameters that are not accessible to other techniques, destructive or non-destructive, and thus offers new insights and complementary information.
Durch den großflächigen Einsatz der Computertomographie (CT) in unterschiedlichen Industriebereichen steigen auch die Anforderungen an die quantitative Bildanalyse. Subjektive Bildwahrnehmung muss durch objektive Algorithmen ersetzt werden. In diesem Artikel stellt die Bundesanstalt für Materialforschung und -prüfung (BAM), die seit den 1980er Jahren an der Entwicklung der industriellen CT beteiligt ist, anhand ausgewählter Beispiele den aktuellen Stand ihrer Analysemethoden an verschiedenen Anwendungsbeispielen der CT vor.
Porous ceramic diesel particulate filters (DPFs) are extruded products that possess macroscopic anisotropic mechanical and thermal properties. This anisotropy is caused by both morphological features (mostly the orientation of porosity) and crystallographic texture. We systematically studied those two aspects in two aluminum titanate ceramic materials of different porosity using mercury porosimetry, gas adsorption, electron microscopy, X-ray diffraction, and X-ray refraction radiography. We found that a lower porosity content implies a larger isotropy of both the crystal texture and the porosity orientation. We also found that, analogous to cordierite, crystallites do align with their axis of negative thermal expansion along the extrusion direction. However, unlike what found for cordierite, the aluminium titanate crystallite form is such that a more pronounced (0 0 2) texture along the extrusion direction implies porosity aligned perpendicular to it.
Among additive manufacturing (AM) technologies, the laser powder bed fusion (L-PBF) is one of the most important technologies to produce metallic components. The layer-wise build-up of components and the complex process conditions increase the probability of the occurrence of defects. However, due to the iterative nature of its manufacturing process and in contrast to conventional manufacturing technologies such as casting, L-PBF offers unique opportunities for in-situ monitoring. In this study, two cameras were successfully tested simultaneously as a machine manufacturer independent process monitoring setup: a high-frequency infrared camera and a camera for long time exposure, working in the visible and infrared spectrum and equipped with a near infrared filter. An AISI 316L stainless steel specimen with integrated artificial defects has been monitored during the build. The acquired camera data was compared to data obtained by computed tomography. A promising and easy to use examination method for data analysis was developed and correlations between measured signals and defects were identified. Moreover, sources of possible data misinterpretation were specified. Lastly, attempts for automatic data analysis by data Integration are presented.
The high-cycle fatigue, small crack propagation behavior of an A357-T6 cast aluminum alloy is investigated. Laboratory X-ray micro-computed tomography (μCT) is used to assist in the manufacturing of two flat fatigue specimens containing subsurface shrinkage pores of different sizes (Pore 1 √A=522μm against Pore 2 √A=280μm). Surface crack monitoring is performed by means of optical microscopy and the cracked specimens are analyzed via scanning electron microscopy and electron backscatter diffraction techniques. The subsurface pores tend to induce intergranular crack nucleation, principally when the grain boundaries are oriented perpendicular to the loading direction. Pore 1 induces a fatigue life reduction of 500.000 cycles when compared to Pore 2. The crystallography is able to influence small crack propagation by slightly decelerating the crack growth rates as well as by altering the crack path topography. Tailoring of the crystallography for improved fatigue resistance requires an investigation of the optimal largest defect to grain size ratio.
Ceramics and their composites are in general brittle materials because they are predominantly made up of ionic and covalent bonds that avoid dislocation motion at room temperature. However, a remarkable ductile behavior has been observed on newly developed 11 mol.% ceria-stabilized zirconia (11Ce-TZP) composite containing fine alumina (8 vol.% Al2O3) and elongated strontium hexa-aluminate (8 vol.% SrAl12O19) grains. The as-synthesized composite also has shown full resistance to Low Temperature Degradation (LTD), relatively high strength and exceptionally high Weibull modulus, allowing its use in a broader range of biomedical applications. In this study, to deepen the understanding of plastic deformation in Ce-TZP based composites that could soon be used for manufacturing dental implants, different mechanical tests were applied on the material, followed by complete microstructural characterization. Distinct from pure Ce-TZP material or other zirconia-based ceramics developed in the past, the material here studied can be permanently strained without affecting the Young modulus, indicating that the ductile response of tested samples cannot be associated to damage occurrence. This ductility is related to the stress-induced tetragonal to monoclinic (t-m) zirconia phase transformation, analogue to Transformation-Induced Plasticity (TRIP) steels, where retained austenite is transformed to martensite. The aim of this study is to corroborate if the observed plasticity can be associated exclusively to the zirconia t-m phase transformation, or also to microcraking induced by the transformation. The t-m transformed-zones produced after bending and biaxial tests were examined by X-ray refraction and SEM/TEM coupled with Raman. The results revealed that the observed elastic-plastic behavior occurs without extensive microcracking, confirming a purely elastic-plastic behavior driven by the phase transformation (absence of damage).
Automatic segmentation of cracks using crack detection methods fails when applied on concrete with embedded reinforcements; it results in artifacts called false-detected cracks. We present a two-step approach to trace the cracks which reduces significantly detecting the false ones. In the first step, the reinforcements were found and removed from the 3D data set, and in the second step, the cracks were detected in the 3D data set free from reinforcements. To visualize and determine the structure and the degree of damages nondestructively, planar tomography as a special case of laminography was used.
While there is a large body of literature on the micro-mechanical behavior of metal matrix composites (MMCs) under uniaxial applied stress, very little is available on multi-phase MMCs. In order to cast light on the reinforcement mechanisms and damage processes in such multi-phase composites, materials made by an Al-based piston alloy and containing one and two ceramic reinforcements (planar-random oriented alumina fibers and SiC particles) were studied. In-situ compression tests during neutron diffraction experiments were used to track the load transfer among phases, while X-ray computed tomography on pre-strained samples was used to monitor and quantify damage. We found that damage progresses differently in composites with different orientations of the fiber mat. Because of the presence of intermetallic network, it was observed that the second ceramic reinforcement changed the load transfer scenario only at very high applied load, when also intermetallic particles break. We rationalized the present results combining them with previous investigations and using a micromechanical model.