Ingenieurwissenschaften und zugeordnete Tätigkeiten
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Young's modulus and Poisson's ratio changes due to machining in porous microcracked cordierite
(2016)
Microstructural changes in porous cordierite caused by machining were characterized using microtensile testing, X-ray computed tomography, and scanning electron microscopy. Young's moduli and Poisson's ratios were determined on similar to 215- to 380-mu m-thick machined samples by combining digital image correlation and microtensile loading. The results provide evidence for an increase in microcrack density and decrease of Young's modulus due to machining of the thin samples extracted from diesel particulate filter honeycombs. This result is in contrast to the known effect of machining on the strength distribution of bulk, monolithic ceramics.
Microstructural changes in porous cordierite for diesel particulate filter applications caused by machining were characterized using microtensile testing and X-ray computed tomography (XCT). Young’s modulus was determined on ~215-380 m thick machined samples by digital image correlation. Results show a decrease of Young’s modulus due to machining of the thin samples. Explanation of this phenomenon was provided by XCT: the presence of debris due to machining and the variation of porosity due to removal of the outer layers were quantified and correlated with the introduction of further microcracking.
X-ray refraction techniques represent a very promising, yet not so wide-spread, set of X-ray techniques
based on refraction effects. They allow determining internal specific surface (surface per unit volume) in a non-destructive fashion, position and orientation sensitive, and with nanometric detectability. While they are limited by the X-ray absorption of the material under investigation, we demonstrate showcases of ceramics and composite materials, where understanding of microstructural features could be achieved in a way unrivalled even by high-resolution techniques such as electron microscopy or computed tomography.
X-ray refraction is analogous to visible light deflection by matter; it occurs at boundaries between different media. The main difference between visible light and X-rays is that in the latter case deflection angles are very small, from a few seconds to a few minutes of arc (i.e., the refraction index n is near to 1). Importantly, deflection of X-rays is also sensitive to the orientation of the object boundaries. These features make X-ray refraction techniques extremely suitable to a) detect defects such as pores and microcracks and quantify their densities in bulk (not too heavy) materials, and b) evaluate porosity and particle properties such as orientation, size, and spatial distribution (by mapping). While X-ray refraction techniques cannot in general image single defects, they can detect objects with size above a few wavelengths of the radiation.
Such techniques, especially at the Synchrotron BESSY II, Berlin, Germany, can be used in-situ, i.e. when the specimen is subjected to temperatures or external loads.
The use of X-ray refraction analysis yields quantitative information, which can be directly input in kinetics, mechanical and damage models.
We hereby show the application of non-destructive X-ray refraction radiography (SXRR, 2D mapping also called topography) to problems in additive manufacturing:
1) Porosity analysis in PBF-LM-Ti64. Through the use of SXRR, we could not only map the (very sparse) porosity distribution between the layers and quantify it, but also classify, and thereby separate, the filled porosity (unmolten powder) from the keyhole and gas pores (Figure 1).
2) In-situ heat treatment of laser powder bed fusion PBF-LM-AlSi10Mg to monitor microstructure and porosity evolution as a function of temperature (Figure 2). By means of SXRR we indirectly observed the initial eutectic Si network break down into larger particles as a function of increasing temperature. We also could detect the thermally induced porosity (TIP). Such changes in the Si-phase morphology upon heating is currently only possible using scanning electron microscopy, but with a much smaller field-of-view. SXRR also allows observing the growth of some individual pores, usually studied via X-ray computed tomography, but again on much smaller fields-of-view.
Our results show the great potential of in-situ SXRR as a tool to gain in-depth knowledge of the defect distribution and the susceptibility of any material to thermally induced damage and/or microstructure evolution over statistically relevant volumes.
In this paper we report on the characterization by X-ray computed tomography of calcium phosphate (CaP) and polycaprolactone (PCL) coatings on Ti-6Al-4V alloy scaffolds used as a material for medical implants. The cylindrical scaffold has greater porosity of the inner part than the external part, thus, mimicking trabecular and cortical bone, respectively. The prismatic scaffolds have uniform porosity. Surface of the scaffolds was modified with calcium phosphate (CaP) and polycaprolactone (PCL) by dip-coating to improve biocompatibility and mechanical properties. Computed tomography performed with X-ray and synchrotron radiation revealed the defects of structure and morphology of CaP and PCL coatings showing small platelet-like and spider-web-like structures, respectively.
In this paper we report on the characterization by X-ray computed tomography of calcium phosphate (CaP) and polycaprolactone (PCL) coatings on Ti-6Al-4V alloy scaffolds used as a material for medical implants. The cylindrical scaffold has greater porosity of the inner part than the external part, thus, mimicking trabecular and cortical bone, respectively. The prismatic scaffolds have uniform porosity. Surface of the scaffolds was modified with calcium phosphate (CaP) and polycaprolactone (PCL) by dip-coating to improve biocompatibility and mechanical properties. Computed tomography performed with X-ray and synchrotron radiation revealed the defects of structure and morphology of CaP and PCL coatings showing small platelet-like and spider-web-like structures, respectively.
The combination of tomographic, microstructural data with other experimental techniques and with modeling is paramount, if we want to extract the maximum amount of information on material and component properties. In particular, quantitative image analysis, statistical approaches, direct discretization of tomographic reconstructions represent concrete possibilities to extend the power of the tomographic 3D representation to insights into the material and component performance. This logic thread equally holds for industrial and academic research and valorizes expensive experiments such as those carried out at synchrotron sources, which cannot be daily repeated.
I will show a few examples of possible use of X-ray tomographic data for quantitative assessment of damage evolution and microstructural properties, as well as for non-destructive testing. Examples of micro-structured inhomogeneous materials will be given, such as Composites, Ceramics, Concrete, and Additively manufactured parts. I will also show how X-ray refraction computed tomography (CT) can be highly complementary to classic absorption CT, being sensitive to internal interfaces.
Additionally, I will show how Neutron Diffraction, which is extremely well suited to the study of internal stresses, both residual and under external load, can well be coupled to the microstructural framework gained by CT, allowing understanding the microstructure-property relationships in materials.
Water migration in one-side heated concrete: 4D in-situ CT monitoring of the moisture-clog-effect
(2019)
Explosive spalling due to fire exposure in concrete structures can lead severe damage and, in the worst case, to premature component failure. For this reason, an in situ investigation of water Migration in concrete due to surface heating was undertaken.
During these experiments, a miniaturized concrete specimen within a confining and insulating double-hull was subjected to surface heating during simultaneous X-ray computed tomography (CT) scanning. Through the use of subtraction-based Image analysis techniques, it was possible to observe and quantify not only drying within areas of the concrete matrix close to the heated surface, but also the migration of moisture to both pore and matrix regions deeper within the specimen. It was also discovered that the correction of CT images for specimen deformation using DVC and variable detector performance using calibrated image filters significantly improved the quality of the results. This clearly demonstrates the potential of X-ray CT for evaluation of other rapid-density-change phenomena in concrete and other building materials.
Abstract While classically used to visualise the magnetic microstructure of functional materials (e.g., for magnetic applications), in this study, the Bitter technique was applied for the first time to visualise macroscopic deformation gradients in a polycrystalline low-carbon steel. Spherical indentation was chosen to produce a multiaxial elastic–plastic deformation state. After removing the residual imprint, the Bitter technique was applied, and macroscopic contrast differences were captured in optical microscopy. To verify this novel characterisation technique, characteristic “hemispherical” deformation zones evolving during indentation were identified using an analytical model from the field of contact mechanics. In addition, near-surface residual stresses were determined experimentally using synchrotron radiation diffraction. It is established that the magnetic domain distribution contrast provides deformation-related information: regions of different domain wall densities correspond to different “hemispherical” deformation zones (i.e., to hydrostatic core, plastic zone and elastic zone, respectively). Moreover, the transitions between these three zones correlate with characteristic features of the residual stress profiles (sign changes in the radial and local extrema in the hoop stress). These results indicate the potential of magnetic domain distribution imaging: visualising macroscopic deformation gradients in fine-grained ferromagnetic material with a significantly improved spatial resolution as compared to integral, mean value-based measurement methods.
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.
Das selektive Laserschmelzen (SLM) ist eine pulverbasierte, additive Fertigungsmethode, welche die Herstellung von komplex und individuell geformten Bauteilen ermöglicht. Im Laufe der vergangenen Jahre haben verschiedene Branchen, unter anderem die Luft- und Raumfahrt Industrie, begonnen diese Technologie intensiv zu erforschen. Insbesondere die Titanlegierung Ti-6Al-V4, welche aufgrund ihrer Kombination von mechanischen Eigenschaften, geringer Dichte und Korrosionsbeständigkeit häufig in der Luft- und Raumfahrt eingesetzt wird, eignet sich für die Herstellung mittels SLM. Allerdings können durch nicht optimal gewählte Prozessparameter, welche für gewöhnlich in einer Energiedichte zusammengefasst werden, Defekte in den Bauteilen entstehen.
In dieser Studie wurde untersucht, in wie weit Röntgen-Refraktionsradiographie geeignet ist diese Defekte zu detektieren und zu charakterisieren. Bei der Röntgen-Refraktionsradiographie wird die Röntgenstrahlung, nachdem sie die Probe transmittiert hat, über einen Analysatorkristall gemäß der Bragg-Bedingung in den 2D-Detektor reflektiert und dabei nach ihrer Ausbreitungsrichtung gefiltert. Dadurch wird neben der Schwächung auch die Ablenkung der Röntgenstrahlung durch Refraktion im inneren der Probe zur Bildgebung ausgenutzt. Aus den aufgenommen Refraktionsradiogrammen kann der Refraktionswert berechnet werden. Dieser ist ein Maß für die Menge an inneren Oberflächen in der Probe.
Zum einen konnte gezeigt werden, dass die Röntgen-Refraktionsradiographie Defekte detektieren kann, die kleiner sind als die Ortsauflösung des verwendeten 2D-Detektors. Zum anderen können zwei verschiedene Typen von Defekten unterschieden werden. Bei dem ersten Typ handelt es sich um runde Poren mit geringer innerer Oberfläche. Diese, sogenannten „keyhole pores“ sind charakteristisch für eine zu hohe Energiedichte während des SLM Prozesses. Bei dem zweiten Typ handelt es sich um nicht komplett aufgeschmolzenes Pulver. Diese Defekte zeichnen sich durch eine hohe innere Oberfläche aus und sind charakteristisch für eine zu geringe Energiedichte. Vergleichende Messungen mit hochauflösender Synchrotron CT und optischer Mikroskopie bestätigen die charakteristischen Formen der verschiedenen Defekte.
The manufacturability of metallic alloys using laser-based additive manufacturing methods such as laser powder bed fusion has substantially improved within the last decade. However, local melting and solidification cause hierarchically structured and crystallographically textured microstructures possessing large residual stress. Such microstructures are not only the origin of mechanical anisotropy but also pose metrological challenges for the diffraction-based residual stress determination. Here we demonstrate the influence of the build orientation and the texture on the microstructure and consequently the mechanical anisotropy of as-built Inconel 718. For this purpose, we manufactured specimens with [001]/[011]-, [001]- and [011]/[111]-type textures along their loading direction. In addition to changes in the Young’s moduli, the differences in the crystallographic textures result in variations of the yield and ultimate tensile strengths. With this in mind, we studied the anisotropy on the micromechanical scale by subjecting the specimens to tensile loads along the different texture directions during in situ neutron diffraction experiments. In this context, the response of multiple lattice planes up to a tensile strain of 10% displayed differences in the load partitioning and the residual strain accumulation for the specimen with [011]/[111]-type texture. However, the relative behavior of the specimens possessing an [001]/[011]- and [001]-type texture remained qualitatively similar. The consequences on the metrology of residual stress determination methods are discussed.
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 triaxial distribution of the residual stress in laser powder bed fused austenitic steel 316L was determined by X-ray and neutron diffraction. The residual stress analysis results were linked to the thermal history of the specimens, which were manufactured with varying inter-layer-times and scanning velocities. A clear link between the in-process temperature of the specimens and the residual stress was found, based on in-situ monitoring data.
Electron Beam Powder Bed Fusion-manufactured (E-PBF) porous components with narrow pores or channels and rough walls or struts can be filled with trapped powder after the manufacturing process. Adequate powder removal procedures are required, especially for high-density porous structures. In the present research, sheetbased porous structures with different thicknesses based on triply periodic minimal surfaces fabricated by EPBF were subjected to different post-processing methods, including a traditional powder recovery system for EPBF, chemical etching and ultrasound vibration-assisted powder removal. Wall thickness, internal defects, microstructure and morphology features, powder distribution inside the specimens, mechanical properties and deformation modes were investigated. A powder recovery system could not remove all residual powder from dense structures. In turn, chemical etching was effective for surface morphology changes and subsurface layers elimination but not for powder removal, as it affected the wall thickness, considerably influencing the mechanical properties of the whole structure. The ultrasound vibration method was quite effective for the removal of residual powder from sheet-based TMPS structures and without a severe degradation of mechanical properties. 10.1016/j.msea.2022.144479 Ultrasound vibration also caused grain refinement.
The stress-induced tetragonal to monoclinic (t-m) zirconia phase transformation can provide a certain degree of plasticity to Ceria-stabilized (Ce-TZP) zirconia-based composites. Characterizing and monitoring this phase transition on a millimeter-size range, within the bulk and in-situ remains a challenge. In this work, the mechanical behavior of Ce-TZP based composite was studied in tension, combining microscopy and synchrotron Xray refraction techniques. In contrast with microscopy methods, which only provide surface information, X-ray refraction radiography (SXRR) allowed the visualization of all the transformation bands, over the entire length and thickness of tested specimens, opening up new avenues for in-situ stress-induced t-m transformation studies.
This study reports on the stress relaxation potential of stress-relieving heat treatments for laser powder bed fused 316L. The residual stress is monitored non-destructively using neutron diffraction before and after the heat treatment. Moreover, the evolution of the microstructure is analysed using scanning electron microscopy. The results show, that a strong relaxation of the residual stress is obtained when applying a heat treatment temperature at 900°C. However, the loss of the cellular substructure needs to be considered when applying this heat treatment strategy.
The safe fatigue design of metallic components fabricated by additive manufacturing (AM) is still a largely unsolved problem. This is primarily due to (a) a significant inhomogeneity of the material properties across the component; (b) defects such as porosity and lack of fusion as well as pronounced surface roughness of the asuilt components; and (c) residual stresses, which are very often present in the as‐built parts and need to be removed by post‐fabrication treatments. Such morphological and microstructural features are very different than in conventionally manufactured parts and play a much bigger role in determining the fatigue life. The above problems require specific solutions with respect to the identification of the critical (failure) sites in AM fabricated components. Moreover, the generation of representative test specimens characterized by similar temperature cycles needs to be guaranteed if one wants to reproducibly identify the critical sites and establish fatigue assessment methods taking into account the effect of defects on crack initiation and early propagation. The latter requires fracture mechanics‐based approaches which, unlike common methodologies, cover the specific characteristics of so‐called short fatigue cracks. This paper provides a discussion of all these aspects with special focus on components manufactured by laser powder bed fusion (L‐PBF). It shows how to adapt existing solutions, identifies fields where there are still gaps, and discusses proposals for potential improvement of the damage tolerance design of L‐PBF components
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 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.