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Eingeladener Vortrag
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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.
Internal damage of an AlSi12CuMgNi alloy reinforced with planar random short fibres has been investigated after compression. This damage strongly influences the load partition between matrix and reinforcement. For fibres perpendicular to the applied load, breakage and interconnected cracks appear in significantly higher volume fraction than with fibres parallel to load.
Load partitioning between phases in a cast AlSi12CuMgNi alloy was investigated by in-situ compression test during neutron diffraction experiments. Computed tomography (CT) was used to determine volume fractions of eutectic Si and intermetallic (IM) phases, and to assess internal damage after ex-situ compression tests. The CT reconstructed volumes showed the interconnectivity of IM phases, which build a 3D network together with eutectic Si. Large stresses were found in IMs, revealing their significant role as a reinforcement for the alloy. An existing micromechanical model based on Maxwell scheme was extended to the present case, assuming the alloy as a three-phase composite (Al matrix, eutectic Si, IM phases). The model agrees well with the experimental data.
Moreover, it allows predicting the principal stresses in each phase, while experiments can only determine stress differences between the axial and radial sample directions. Finally, we showed that the addition of alloying elements not only allowed developing a 3D interconnected network, but also improved the strength of the Al matrix, and the ability of the alloy constituents to bear mechanical load.
The influence of the support structure on residual stress and distortion in SLM Inconel 718 parts
(2018)
The effect of support structure and of removal from the base plate on the residual stress state in selective laser melted IN718 parts was studied by means of synchrotron X-ray diffraction. The residual stresses in subsurface region of two elongated prisms in as-built condition and after removal from the base plate were determined. One sample was directly built on a base plate and another one on a support structure. Also, the distortion on the top surface due to stress release was measured by contact profilometry. High tensile residual stress values were found, with pronounced stress gradient along the hatching direction. In the sample on support, stress redistribution took place after removal from the base plate, as opposed to simple stress relaxation for the sample without support. The sample on support structure showed larger distortion compared to sample without support. We conclude that the use of a support decreases stress values but stress-relieving heat treatments are still needed.
The residual stress (RS) in laser powder bed fusion (LPBF) IN718 alloy samples produced using a 67°-rotation scan strategy is investigated via laboratory X-ray diffraction (XRD) and neutron diffraction (ND). The location dependence of the strain-free (d₀) lattice spacing in ND is evaluated using a grid array of coupons extracted from the far-edge of the investigated specimen. No compositional spatial variation is observed in the grid array. The calculated RS fields show considerable non-uniformity, significant stress gradients in the region from 0.6 to 2 mm below the surface, as well as subsurface maxima that cannot be accounted for via XRD. It is concluded that failure to determine such maxima would hamper a quantitative determination of RS fields by means of the stress balance method.
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.
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.
Although layer-based additive manufacturing methods such as laser powder bed fusion (PBF-LB) offer an immense geometrical freedom in design, they are typically subject to a build-up of internal stress (i.e. thermal stress) during manufacturing. As a consequence, significant residual stress (RS) is retained in the final part as a footprint of these internal stresses. Furthermore, localized melting and solidification inherently induce columnar-type grain growth accompanied by crystallographic texture. Although diffraction-based methods are commonly used to determine the RS distribution in PBF-LB parts, such features pose metrological challenges in their application. In theory, preferred grain orientation invalidates the hypothesis of isotropic material behavior underlying the common methods to determine RS. In this work, more refined methods are employed to determine RS in PBF-LB/M/IN718 prisms, based on crystallographic texture data. In fact, the employment of direction-dependent elastic constants (i.e. stress factors) for the calculation of RS results in insignificant differences from conventional approaches based on the hypothesis of isotropic mechanical properties. It can be concluded that this result is directly linked to the fact that the {311} lattice planes typically used for RS analysis in nickel-based alloys have high multiplicity and less strong texture intensities compared with other lattice planes. It is also found that the length of the laser scan vectors determines the surface RS distribution in prisms prior to their removal from the baseplate. On removal from the baseplate the surface RS considerably relaxes and/or redistributes; a combination of the geometry and the scanning strategy dictates the sub-surface RS distribution.
Im vergangenen Jahrzehnt sind gitterinterferometrische Röntgenabbildungen zunehmend in den Fokus des Interesses gerückt. Sie sind insbesondere dann Vorteil, wenn der in der Standardradiographie erreichbare Kontrast nicht genügt, schwach absorbierende Mikro- und Nanostrukturen abzubilden.
Auf Kosten mehrerer Aufnahmen gestattet die Talbot-Lau Gitterinterferometrie, die Beiträge aus Absorption, Refraktion und (refraktiver) Streuung zu trennen. Dazu werden die Störungen der Interferenzmuster von Phasengittern ausgewertet. Im Gegensatz zu einer Vielzahl anderer refraktionsbasierter Abbildungsmethoden kann diese Technik mit konventionellen Röntgenröhren (mit divergenter, polychromatischer Strahlung) angewendet werden. Damit ist die Technik geeignet, typische ZfP-Fragestellungen zu lösen.
Hier stellen wir Untersuchungen zur Effizienz von Phasengittern vor. Die Visibilität (d.h. die Höhe der Oszillation im Interferenzmuster) wird als Funktion verschiedener geometrischer Parameter verfolgt. Eine Rotation um die Achse parallel zu den Gitterstegen ändert die Form des Gitterprofils (d.h. die Verteilung der Phasenschiebungen). Die kontinuierliche Variation des Winkels und des Detektionsabstandes führt zur Identifikation von ausgezeichneten Kombinationen mit maximaler Visibilität, wobei die Abstände deutlich geringer sind als im Standardaufbau mit senkrechter Gitterbestrahlung.
Unsere Studie umfasst Simulationen für monochromatische Quelle und den Vergleich zu experimentellen Ergebnissen mit der Synchrotronstrahlung.
In der Literatur wurden die Vorteile der Talbot-Lau Interferometrie für die zerstörungsfreie Prüfung von Faserkompositen und Verbundwerkstoffen demonstriert. Hier werden als Beispiele Messungen an Aluminiumtitanat (Al2TiO5) Pulver gezeigt.
Grating interferometric set-ups have been established in the last decade. They are promising candidates to obtain enhanced image contrast from weakly absorbing micro and nano structures. They are based on X-ray refraction and near-field diffraction using the Talbot effect.
At the expense of taking multiple images, Talbot-Lau grating interferometry allows separating the absorption, refraction, and scattering contributions by analysing the disturbances of a phase grating interference pattern. Contrary to other refraction enhanced methods, this technique can be applied using conventional X-ray tubes (divergent, polychromatic source). This makes it attractive to solve typical non-destructive testing problems.
We investigated the efficiency of phase gratings, i.e. the visibility (the amplitude of oscillations) upon variation of propagation distance and phase grating rotation around an axis parallel to the grid lines. This grating rotation changes the grating shape (i.e. the distributions of phase shifts). This can yield higher visibilities than derived from rectangular shapes.
Our study includes experimental results obtained from synchrotron radiation, as well as simulations for monochromatic radiation. The advantages of Talbot-Lau interferometry are demonstrated at the example of glass capillaries.
Grating interferometric set-ups have been established in the last decade. They are promising candidates to obtain enhanced image contrast from weakly absorbing micro and nano structures. They are based on X-ray refraction and near-field diffraction using the Talbot effect.
At the expense of taking multiple images, Talbot-Lau grating interferometry allows separating the absorption, refraction, and scattering contributions by analysing the disturbances of a phase grating interference pattern. Contrary to other refraction enhanced methods, this technique can be applied using conventional X-ray tubes (divergent, polychromatic source). This makes it attractive to solve typical non-destructive testing problems.
We investigated the efficiency of phase gratings, i.e. the visibility (the amplitude of oscillations) upon variation of propagation distance and phase grating rotation around an axis parallel to the grid lines. This grating rotation changes the grating shape (i.e. the distributions of phase shifts). This can yield higher visibilities than derived from rectangular shapes.
Our study includes experimental results obtained from synchrotron radiation, as well as simulations for monochromatic radiation. The advantages of Talbot-Lau interferometry are demonstrated at the example of glass capillaries.
For the first time, synchrotron X-ray refraction radiography (SXRR) has been paired with in-situ heat treatment to monitor microstructure and porosity evolution as a function of temperature. The investigated material was a laser powder bed fusion (LPBF) manufactured AlSi10Mg, where the initial eutectic Si network is known to disintegrate and spherodize into larger particles with increasing temperature. Such alloy is also prone to thermally induced porosity (TIP). We show that SXRR allows detecting the changes in the Si-phase morphology upon heating, while this is currently possible only using scanning electron microscopy. SXRR also allows observing the growth of pores, usually studied via X-ray computed tomography, but 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 susceptibility of any material to thermally induced damage and/or microstructure evolution over statistically relevant volumes.
Synchrotron X-ray diffraction is a powerful non-destructive technique for the analysis of the material stress-state. High cooling rates and heterogeneous temperature distributions during additive manufacturing lead to high residual stresses. These high residual stresses play a crucial role in the ability to achieve complex geometries with accuracy since they can promote distortion of parts during manufacturing. Furthermore, residual stresses are critical for the mechanical performance of parts in terms of durability and safety.
In the present study, Ti-6Al-4V bridge-like specimens were manufactured additively by selective laser melting (SLM) under different laser scanning speed conditions in order to compare the effect of process energy density on the residual stress state. Subsurface residual stress analysis was conducted by means of synchrotron X-ray diffraction in energy dispersive mode for three conditions: as-built on base plate, released from base plate, and after heat treatment on the base plate. The quantitative residual stress characterization shows a correlation with the qualitative bridge curvature method. Computed tomography (CT) was carried out to ensure that no stress relief took place owing to the presence of porosity. CT allows obtaining spatial and size pores distribution which helps in optimization of the SLM process.
High tensile residual stresses were found at the lateral surface for samples in the as-built conditions. We observed that higher laser energy density during fabrication leads to lower residual stresses. Samples in released condition showed redistribution of the stresses due to distortion.
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.
In order to investigate their microcracking behaviour, the microstructures of several β-eucryptite ceramics, obtained from glass precursor and cerammed to yield different grain sizes and microcrack densities, were characterized by laboratory and synchrotron x-ray refraction and tomography. Results were compared with those obtained from scanning electron microscopy (SEM). In SEM images, the characterized materials appeared fully dense but computed tomography showed the presence of pore clusters. Uniaxial tensile testing was performed on specimens while strain maps were recorded and analyzed by Digital Image Correlation (DIC). X-ray refraction techniques were applied on specimens before and after tensile testing to measure the amount of the internal specific surface (i.e., area per unit volume). X-ray refraction revealed that (a) the small grain size (SGS) material contained a large specific surface, originating from the grain boundaries and the interfaces of TiO2 precipitates; (b) the medium (MGS) and large grain size (LGS) materials possessed higher amounts of specific surface compared to SGS material due to microcracks, which decreased after tensile loading; (c) the precursor glass had negligible internal surface. The unexpected decrease in the internal surface of MGS and LGS after tensile testing is explained by the presence of compressive regions in the DIC strain maps and further by theoretical arguments. It is suggested that while some microcracks merge via propagation, more close mechanically, thereby explaining the observed X-ray refraction results. The mechanisms proposed would allow the development of a strain hardening route in ceramics.
Stress-induced damage evolution in cast AlSi12CuMgNi alloy with one- and two ceramic reinforcements
(2017)
Two composites, consisting of an as-cast AlSi12CuMgNi alloy reinforced with 15%vol. Al2O3 short fibres and with 7%vol. Al2O3 short fibres + 15%vol. SiC particles were studied. Synchrotron computed tomography disclosed distribution, orientation, and volume fraction of the different phases. In-situ compression tests during neutron diffraction in direction parallel to the fibres plane revealed the load partition between phases. Internal damage (fragmentation) of the Si phase and Al2O3 fibres was directly observed in CT reconstructions. Significant debonding between Al-matrix and SiC particles was also found. Finally, based on the Maxwell scheme, a micro-mechanical model was utilized for the new composite with two ceramic reinforcements; it rationalizes the experimental data, and predicts the evolution of all internal stress components in each phase.
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.
Electron backscatter diffraction (EBSD) images of extruded pure aluminum were statistically analyzed to investigate creep-induced subgrain structures after applying two different levels of creep stress, corresponding to the power law (PL) and power-law breakdown (PLB) regimes. Kernel average misorientation analysis of EBSD measurements revealed 2D morphologies, which were subdivided by a multi-step segmentation procedure into subgranular arrangements. Various descriptors were employed to characterize the “subgrains” quantitatively, including their size, shape, spatial arrangement, and crystallographic orientation. In particular, the analysis of the orientations of subgrains was conducted by neglecting rotations around the loading axis. This approach facilitated the individual investigation of the {001} and {111} subgrain families with respect to the loading axis for two investigated stress levels plus a reference specimen. For the PL regime, the statistical analysis of subgrain descriptors computed from segmented image data revealed a similar degree of strain accumulation for {111} and {001} subgrains. In contrast, for the PLB regime, the analyzed descriptors indicate that {111} subgrains tend to accumulate significantly more strain than {001} ones. These observations suggest that the mechanisms leading to PLB may be associated with strain localization dependent on intergranular stress, hindering the recovery process within {111} grains.
While additive manufacturing (AM) is blossoming in nearly every industrial field, and the most different process are being used to produce components and materials, little attention is paid on the safety concerns around AM materials and processes.
Leveraging on our leading expertise in non-destructive testing (NDT) and materials characterization, we approach AM at BAM under two important viewpoints: first the on-line monitoring of the process and of the product, second the evolution of the (unstable) microstructure of AM materials under external loads.
These two subjects are the core of the two new-born internal projects ProMoAM and AGIL, respectively.
A detailed view of the goals and the organization of these two projects will be given, together with the expected output, and some preliminary results.
Large temperature gradients inherent to additive manufacturing (AM) processes induce large residual stress (RS) in the final part. Because RS can influence the tribological properties, this study focuses on the relationship between wear sliding properties and RS in IN718 coatings. Such coatings were deposited with a Laser metal deposition (LMD) machine using two different scanning strategies.
The wear resistance and RS state were investigated after surface milling. RS were measured before and after wear tests on a reciprocating sliding test apparatus.
Two different X-ray diffraction techniques were employed to measure the surface and subsurface state RS: Laboratory Energy Dispersive X-ray Diffraction (LEDXD) and Synchrotron X-ray Energy Dispersive Diffraction (SXEDD). Due to the milling process, the coatings show similar depth distributions of RS from 22 to 92 μm depth, but exhibit different magnitudes depending on the scanning strategy used. Reciprocating sliding wear tests induced high compressive residual stresses that erased the initial RS state, and a similar wear behavior was observed in the two samples. These samples possess similar texture and grain morphology. This demonstrates that the influence of RS on wear resistance is a second-order effect. Nevertheless, it was observed that RS can still impact the wear performance at the early testing stages of the repaired parts.
Manufacturing defects, high residual stress (RS), and microstructures affect the structural integrity of laser powder bed fusion (LPBF) Ti-6Al-4V. In this study, the individual effect of these factors on fatigue performance at elevated temperature (300 °C) was evaluated. Material in as-built condition and subjected to post-processing, including two heat treatments and hot isostatic pressing, was investigated. It was found that in the absence of tensile RS, the fatigue life at elevated temperature is primary controlled by the defects; and densification has a much stronger effect than the considered heat treatments on the improvement of the mechanical performance.
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.
Additive manufacturing (AM) is developing rapidly due to itsflexibility in producing complex geometries and tailored material compositions. However, AM processes are characterized by intrinsic limitations concerning their resolution and surface finish, which are related to the layer-by-layer stacking process. Herein, a self-organization process is promoted as an approach to improve surface quality and achieve optimization of 3D minimal surface lightweight structures. The self-organization is activated after the powder bed 3D printing process via local melting, thereby allowing surface tension-driven viscous flow.The surface roughness Ra (arithmetic average of the roughness profile) could bedecreased by a factor of 1000 and transparent lenses and complex gyroid structures could be produced for demonstration. The concept of self-organization is further elaborated by incorporating external magnetic fields to intentionally manipulate magnetic particles, which are mixed with the polymer before printing and self-organization. This concept can be applied to develop programmable materials with specific microtextures responding to the external physical conditions.
Scanning Manufacturing Parameters Determining the Residual Stress State in LPBF IN718 Small Parts
(2021)
The influence of scan strategy on the residual stress (RS) state of an as-built IN718 alloy produced by means of laser powder bed fusion (LPBF) is investigated. Two scan vector rotations (90°-alternation and 67°-rotation), each produced following two different scan vector lengths (long and short), are used to manufacture four rectangular prisms. Neutron diffraction (ND) and laboratory X-ray diffraction (XRD) techniques are used to map the bulk and surface RS state, respectively. The distortion induced upon removal from the baseplate is measured via profilometry. XRD measurements show that the two long scan vector strategies lead to higher RS when compared with the equivalent short scan vector strategies. Also, the 67°-rotation strategies generate lower RS than their 90°-alternation counterparts. Due to the lack of reliable stress-free d0 references, the ND results are analyzed using von Mises stress. In general, ND results show significant RS spatial non-uniformity. A comparison between ND and distortion results indicates that the RS component parallel to the building direction (Z-axis) has a predominant role in the Z-displacement. The use of a stress balance scheme allows to discuss the d0 variability along the length of the specimens, as well as examine the absolute RS state.
Additiv gefertigte (AM) dreifach periodische metallische minimale Oberflächenstrukturen (TPMSS, aus dem Englischen Triply Periodic Minimum Surface Structures) erfüllen mehrere Anforderungen sowohl im biomedizinischen als auch im technischen Bereich: Abstimmbare mechanische Eigenschaften, geringe Empfindlichkeit gegenüber Herstellungsfehlern, mechanische Stabilität und hohe Energieabsorption. Allerdings stellen sie auch einige Herausforderungen in Bezug auf die Qualitätskontrolle dar, die ihre erfolgreiche Anwendung verhindern können. Tatsächlich ist die Optimierung des AM-Prozesses ohne die Berücksichtigung struktureller Merkmale wie Fertigungsgenauigkeit, interne Defekte sowie Oberflächentopographie und -rauheit unmöglich. In dieser Studie wurde die quantitative zerstörungsfreie Analyse von Ti-6Al-4V-Legierung TPMSS mit Hilfe der Röntgen-Computertomographie (XCT) durchgeführt. Es werden mehrere neue Bildanalyse-Workflows vorgestellt, um die Auswirkungen der Aufbaurichtung auf die Wanddickenverteilung, die Wanddegradation und die Verringerung der Oberflächenrauheit aufgrund des chemischen Ätzens von TPMSS zu bewerten. Es wird gezeigt, dass die Herstellungsgenauigkeit für die Strukturelemente, die parallel und orthogonal zu den hergestellten Schichten gedruckt werden, unterschiedlich ist. Verschiedene Strategien für das chemische Ätzen zeigten unterschiedliche Pulverabtragsfähigkeiten und damit ein Gradient der Wanddicke. Dies wirkte sich auf die mechanische Leistung unter Druck durch die Verringerung der Streckspannung aus. Eine positive Auswirkung des chemischen Ätzens ist die Verringerung der Oberflächenrauhigkeit, die möglicherweise die Ermüdungseigenschaften der Bauteile verbessern kann. Schließlich wurde XCT eingesetzt, um die Menge des zurückgehaltenen Pulvers mit der Porengröße des TPMSS zu korrelieren, wodurch der Herstellungsprozess weiter verbessert werden kann.
Wir präsentieren Labor- und Synchrotron-Röntgenrefraktionstechniken, wie sie an der BAM implementiert sind.
Wir zeigen, dass die Labor-Röntgenrefraktionstopographie (XRRT) und die Synchrotron-Röntgenrefraktionsradiographie (SRRR) außergewöhnliche Werkzeuge zur Untersuchung von Schädigungen und inneren Defekten (Poren, Mikrorisse) in leichten Materialien wie Keramiken und Kompositen sind. Tatsächlich nutzen diese Techniken den an Grenzflächen auftretenden Röntgenbrechungseffekt aus, um den Kontrast zwischen dem (schwach absorbierenden) Objekt und dem Hintergrund zu erhöhen. Dies ermöglicht die Erkennung sehr kleiner Objekte (sogar bis zu 1 nm Rissöffnung) und die Quantifizierung ihrer spezifischen Oberfläche, die mit ihrem Einfluss auf die Materialeigenschaften korreliert. Wir zeigen die folgenden Anwendungen: a) Quantifizierung der Faserentbindung in laminaten Epoxid-Kohlenstoff-Verbundwerkstoffen; b) Mapping der Porengröße in gesinterten Keramiken; c) Eindringstiefe von Aschen in Keramikschutzschichten; d) Quantifizierung der Porenorientierung in Diesel Partikelfiltern; e) 3D-Darstellung von Makrorissen und Faserentbindung in Verbundwerkstoffen auf Ti-Basis für Anwendungen in der Luft- und Raumfahrt (unter Verwendung von Röntgenrefraktionstomographie).
In Leichtbauanwendungen sind Materialien mit geringen Dichten und hohen Festigkeiten gefragt. Insbesondere Faser-Kunststoff-Verbunde (FKV) erfüllen diese Anforderungen und werden zunehmend für Strukturbauteile eingesetzt. Die Oberflächen moderner Rotorblätter von Windkraftanlagen werden aus FKV gefertigt. Das Versagen dieser Materialien hat massiven Einfluss auf die Einsatzfähigkeit der gesamten Windkraftanlage. Daher ist die Kenntnis des Versagensverhaltens dieser Komponenten unter statischer und zyklischer Belastung von großem Interesse, um die Betriebsbeanspruchung abzuschätzen. Im Idealfall wird die Schadensentwicklung unter Betriebslast mit zerstörungsfreien in-situ-Prüfverfahren ermittelt. Hier berichten wir über die Beobachtung der Rissentwicklung in Carbon-Faserverstärkten Kunststoffen (CFK) unter kontinuierlicher Zugbelastung durch in-situ Synchrotron-Röntgenrefraktionsradiographie. Eine selbst entwickelte elektromechanische Zugprüfmaschine mit einem Kraftbereich bis zu 15 kN wurde in den Strahlengang an der BAMline (BESSY II) integriert. Da in herkömmlichen (Absorptions-) Radiographien Defekte wie Zwischenfaserbrüche oder Faser-Matrix-Enthaftung keinen ausreichenden Kontrast verursachen, wird zur Kontrastanhebung die Röntgenrefraktion benutzt. Hier wird das sogenannte Diffraction Enhanced Imaging (DEI) angewandt, um Primär- und gebrochene Strahlung mit Hilfe eines Analysatorkristalls zu trennen. Diese Technik ermöglicht schnelle Messungen mit einem Gesichtsfeld von einigen Quadratmillimetern (hier: 14 mm × 7.2 mm) und ist ideal für in-situ Untersuchungen. Die Bildgebung und der Zugversuch erfolgen mit einer Bildfrequenz von 0.7 / s und einer Dehnrate von 0.00055 / s . Bei 0°/90° Fasergelegen treten die ersten Zwischenfaserrisse bei 380 MPa (Dehnung 0.8 %) auf. Vor dem Versagen bei ca. 760 MPa (Dehnung 2.0 %) beobachten wir die Ausbildung eines nahezu äquidistanten Rissmusters (Risse in ca. 1 mm Abstand), das sich im geschädigten Zustand über die gesamte Probe erstreckt.
Additive Manufacturing (AM) through the Selective Laser Melting (SLM) route offers ample scope for producing geometrically complex parts compared to the conventional subtractive manufacturing strategies. Nevertheless, the residual stresses which develop during the fabrication can limit application of the SLM components by reducing the load bearing capacity and by inducing unwanted distortion, depending on the boundary conditions specified during manufacturing. The present study aims at characterizing the residual stress states in the SLM parts using different diffraction methods. The material used is the nickel based superalloy Inconel 718. Microstructure as well as the surface and bulk residual stresses were characterized. For the residual stress analysis, X-ray, synchrotron and neutron diffraction methods were used. The measurements were performed at BAM, at the EDDI beamline of -BESSY II synchrotronand the E3 line -BER II neutron reactor- of the Helmholtz-Zentrum für Materialien und Energie (HZB) Berlin. The results reveal significant differences in the residual stress states for the different characterization techniques employed, which indicates the dependence of the residual state on the penetration depth in the sample. For the surface residual stresses, longitudinal and transverse stress components from X-ray and synchrotron agree well and the obtained values were around the yield strength of the material. Furthermore, synchrotron mapping disclosed gradients along the width and length of the sample for the longitudinal and transverse stress components. On the other hand, lower residual stresses were found in the bulk of the material measured using neutron diffraction. The longitudinal component was tensile and decreased towards the boundary of the sample. In contrast, the normal component was nearly constant and compressive in nature. The transversal component was almost negligible. The results indicate that a stress re-distribution takes place during the deposition of the consecutive layers. Further investigations are planned to study the phenomenon in detail.
The influence of the process gas, laser scan speed, and sample thickness on the build-up of residual stresses and porosity in Ti-6Al-4V produced by laser powder bed fusion was studied. Pure argon and helium, as well as a mixture of those (30% helium), were employed to establish process atmospheres with a low residual Oxygen content of 100 ppm O2. The results highlight that the subsurface residual stresses measured by X-ray diffraction were significantly lower in the thin samples (220 MPa) than in the cuboid samples (645 MPa). This difference was attributed to the shorter laser vector length, resulting in heat accumulation and thus in-situ stress relief. The addition of helium to the process gas did not introduce additional subsurface residual stresses in the simple geometries, even for the increased scanning speed. Finally, larger deflection was found in the cantilever built under helium (after removal from the baseplate), than in those produced under argon and an argon-helium mixture. This result demonstrates that complex designs involving large scanned areas could be subjected to higher residual stress when manufactured under helium due to the gas’s high thermal conductivity, heat capacity, and thermal diffusivity.
The residual stress distribution in IN718 elongated prisms produced by Selective Laser Melting was studied by means of neutron (bulk) and laboratory X-ray (surface) diffraction.
Two deposition hatch lengths were considered. A horizontal plane near the top surface (perpendicular to the building direction) and a vertical plane near the lateral surface (parallel to the building direction) were investigated. Samples both in as-built (AB) condition and removed (RE) from the base plate were characterized.
While surface stress fields seem constant for AB condition, X-ray diffraction shows stress gradients along the hatch direction in the RE condition. The stress profiles correlate with the distortion maps obtained by tactile probe measurements.
Neutron diffraction shows bulk stress gradients for all principal components along the main sample directions. We correlate the observed stress patterns with the hatch length, i.e. with its effect on temperature gradients and heat flow. The bulk stress gradients partially disappear after removal from the baseplate.
The residual stress distribution of tungsten inert gas welded S235JRC+C plates was determined by means of neutron diffraction(ND). Large longitudinal residual stresses with maxima around 600 MPa were found. With these results as reference, the evaluation of residual stress with high spatial resolution GMR (giant magneto resistance) sensors was discussed. The experiments performed indicate a correlation between changes in residual stresses (ND) and the normal component of local residual magnetic stray fields (GMR). Spatial variations in the magnetic field strength perpendicular to the welds are in the order of the magnetic field of the earth.
We investigated the possibility of minimizing tensile matrix residual stresses in age hardenable aluminum alloy metal matrix composites without detrimentally affect their mechanical properties (such as yield strength).
Specifically, we performed thermal treatments at different temperatures and times in an age-hardenable aluminum matrix composite 2014Al-15vol%Al2O3. Using X-ray synchrotron radiation diffraction and mechanical tests, we show that below a certain treatment temperature (250 °C) it is possible to identify an appropriate thermal treatment capable of relaxing residual stress in this composite while even increasing its yield strength, with respect to the as processed conditions.
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.
While the problem of the identification of mechanisms of hydrogen assisted damage has and is being thoroughly studied, the quantitative analysis of such damage still lacks suitable tools. In fact, while, for instance, electron microscopy yields excellent characterization, the quantitative analysis of damage requires at the same time large field-of-views and high spatial resolution. Synchrotron X-ray refraction techniques do possess both features. In this work, we show how synchrotron X-ray refraction computed tomography (SXRCT) can quantify damage induced by hydrogen embrittlement in a lean duplex steel, yielding results that overperform even those achievable by synchrotron X-ray absorption computed tomography. As already reported in literature, but this time using a non-destructive technique, we show that the hydrogen charge does not penetrate to the center of tensile specimens. By the comparison between virgin and hydrogen-charged specimens, we deduce that cracks in the specimen bulk are due to the rolling process rather than hydrogen-assisted. We show that (micro)cracks propagate from the surface of tensile specimens to the interior with increasing applied strain, and we deduce that a significant crack propagation can only be observed short before rupture.
The most substantial innovations in radiographic imaging techniques of the last two decades aim at enhanced image contrast of weakly absorbing micro and nano structures by taking advantage of X-ray refraction effects occurring at outer and inner surfaces. The applications range from fibre reinforced plastics to biological tissues. These techniques comprise, among others, X-ray refraction topography, diffraction enhanced imaging, phase contrast imaging, Talbot-Lau grating interferometry, and refraction enhanced imaging. They all make use of selective beam deflections up to a few minutes of arc: the X-ray refraction effect. In contrast to diffraction, this type of interaction has a 100 % scattering cross section, as shown experimentally. Since X-ray refraction is very sensitive to the orientation of interfaces, it is additionally a tool to detect, e.g., fibre or pore orientation. If the detector resolution exceeds the size of (small) individual features, one detects the integral information (of inner surfaces) within the gauge volume. We describe the above-mentioned techniques, and show their experimental implementation in the lab and at a synchrotron source. We also show strategies for data processing and quantitative analysis.
Additively manufactured (AM) metallic sheet-based Triply Periodic Minimal Surface Structures (TPMSS) meet several requirements in both bio-medical and engineering fields: Tunable mechanical properties, low sensitivity to manufacturing defects, mechanical stability, and high energy absorption. However, they also present some challenges related to quality control. In fact, the optimization of both the AM process and the properties of TPMSS is impossible without considering structural characteristics as manufacturing accuracy, internal defects, and as well as surface topography and roughness. In this study, the quantitative non-destructive analysis of TPMSS manufactured from Ti-6Al-4V alloy by electron beam melting was performed by means of laboratory X-ray computed tomography (XCT).
Additively manufactured (AM) triply periodic metallic minimum surface structures (TPMSS, from the English Triply Periodic Minimum Surface Structures) fulfill several requirements in both biomedical and engineering fields: tunable mechanical properties, low sensitivity to manufacturing defects, mechanical stability, and high energy absorption. However, they also present some quality control challenges that may prevent their successful application. In fact, optimization of the AM process is impossible without considering structural features such as manufacturing accuracy, internal defects, and surface topography and roughness. In this study, quantitative nondestructive analysis of Ti-6Al-4V alloy TPMSS was performed using X-ray computed tomography (XCT). Several new image analysis workflows are presented to evaluate the effects of buildup direction on wall thickness distribution, wall degradation, and surface roughness reduction due to chemical etching of TPMSS. It is shown that the fabrication accuracy is different for the structural elements printed parallel and orthogonal to the fabricated layers. Different strategies for chemical etching showed different powder removal capabilities and thus a gradient in wall thickness. This affected the mechanical performance under compression by reducing the yield stress. A positive effect of chemical etching is the reduction of surface roughness, which can potentially improve the fatigue properties of the components. Finally, XCT was used to correlate the amount of powder retained with the pore size of the TPMSS, which can further improve the manufacturing process.
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).
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.
Porous ceramic diesel particulate filters (DPFs) are extruded products that possess macroscopic anisotropic mechanical and thermal properties. This anisotropy is caused by both morphologic features (mostly the orientation of porosity) and crystallographic texture. We systematically studied those two aspects in a cordierite and two aluminum titanate (AT) 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 in AT content implies a larger isotropy of both the crystal texture and the porous space orientation. We also found that, analogous to cordierite, AT 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.
The performance of grating interferometers coming up now for Imaging interfaces within materials depends on the efficiency (visibility) of their main component, namely the phase grating. Therefore, experiments with monochromatic synchrotron radiation and corresponding simulations are carried out. The visibility of a Phase grating is optimized by different photon energies, varying detector to grating distances and continuous rotation of the phase grating about the grid lines. Such kind of rotation changes the projected grating shapes, and thereby the distribution profiles of phase shifts. This yields higher visibilities than derived from ideal rectangular shapes. By continuous grating rotation and variation of the propagation distance, we achieve 2D visibility maps. Such maps provide the visibility for a certain combination of grating orientation and detector position. Optimum visibilities occur at considerably smaller distances than in the standard setup.
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 detection of internal irregularities is crucial for quality assessment in metal-based additive manufacturing (AM) technologies such as laser powder bed fusion (L-PBF). The utilization of in-process thermography as an in situ monitoring tool in combination with post-process X-ray micro computed tomography (XCT) as a reference technique has shown great potential for this aim. Due to the small irregularity dimensions, a precise registration of the datasets is necessary as a
requirement for correlation. In this study, the registration of thermography and XCT reference datasets of a cylindric specimen containing keyhole pores is carried out for the development of a porosity prediction model. The considered datasets show variations in shape, data type and dimensionality, especially due to shrinkage and material elevation effects present in the manufactured part. Since the resulting deformations are challenging for registration, a novel preprocessing methodology is introduced that involves an adaptive volume adjustment algorithm which is based on the porosity distribution in the specimen. Thus, the implementation of a simple three-dimensional image-to-image registration is enabled. The results demonstrate the influence of the part deformation on the resulting porosity location and the importance of registration in terms of irregularity prediction.
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.
A range of heat treatments have been developed for wrought Inconel 718 to obtain desired properties. For additively manufactured Inconel 718, the recently developed standard ASTM F3301 provides guidance for heat treatment of powder bed fusion specimens. Although this standard is based on standards developed for wrought Inconel 718, it does not include direct aging. Since direct aging reduces the number of processing steps, it can result in a post processing cost reduction if the desired properties are obtained. In this study, we characterized the microstructure and tensile behavior of Inconel 718 specimens produced by a laser powder bed fusion process. The specimens were heat treated according to two different routines after stress relieving: a full heat Treatment versus a one-step direct aging process. Differences in the resulting texture and grain morphology were observed.
The ex-situ stress-strain behavior was broadly similar. However, a slight increase in yield strength was observed for the direct aged specimen. In order to understand this behavior, investigations with in-situ synchrotron Energy dispersive X-ray diffraction tensile testing revealed differences in the load partitioning among different Crystal directions. Importantly, the elastic anisotropy expressed by the magnitude of the diffraction elastic constants showed a dependency on the microstructures.
The determination of residual stresses becomes more complicated with increasing complexity of the structures investigated. Additive manufacturing techniques generally allow the production of ‘lattice structures’ without any additional manufacturing step. These lattice structures consist of thin struts and are thus susceptible to internal stress-induced distortion and even cracks. In most cases, internal stresses remain locked in the structures as residual stress.
The determination of the residual stress in lattice structures through nondestructive neutron diffraction is described in this work. It is shown how two difficulties can be overcome: (a) the correct alignment of the lattice structures within the neutron beam and (b) the correct determination of the residual stress field in a representative part of the structure. The magnitude and the direction of residual stress are discussed. The residual stress in the strut was found to be uniaxial and to follow the orientation of the strut, while the residual stress in the knots was more hydrostatic. Additionally, it is shown that strain measurements in at least seven independent directions are necessary for the estimation of the principal stress directions. The measurement directions should be chosen according to the sample geometry and an informed choice on the possible strain field. If the most prominent direction is not measured, the error in the calculated stress magnitude increases considerably.
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.
A numerical framework is developed to study the hysteresis of elastic properties of porous ceramics as a function of temperature. The developed numerical model is capable of employing experimentally measured crystallographic orientation distribution and coefficient of thermal expansion values. For realistic modeling of the microstructure, Voronoi polygons are used to generate polycrystalline grains. Some grains are considered as voids, to simulate the material porosity. To model intercrystalline cracking, cohesive elements are inserted along grain boundaries. Crack healing (recovery of the initial properties) upon closure is taken into account with special cohesive elements implemented in the commercial code ABAQUS. The numerical model can be used to estimate fracture properties governing the cohesive behavior through inverse analysis procedure. The model is applied to a porous cordierite ceramic. The obtained fracture properties are further used to successfully simulate general non-linear macroscopic stress-strain curves of cordierite, thereby validating the model.
This paper focuses on the aspect on how damage evolution processes in composite materials and structures including matrix fracture, delamination, fibre-matrix debonding, and fibre fracture can be detected by taking advantage of the material’s inherit mechanical properties. These properties can be described on the basis of non-linear mechanical phenomena measurable as an inert frequency response signal. The approach is proposed as a means for residual life structural assessment specifically in the context of VHCF.
While the volumetric energy density is commonly used to qualify a process parameter set, and to quantify its influence on the microstructure and performance of additively manufactured (AM) materials and components, it has been already shown that this description is by no means exhaustive. In this work, new aspects of the optimization of the selective laser melting process are investigated for AM Ti-6Al-4V. We focus on the amount of near-surface residual stress (RS), often blamed for the failure of components, and on the porosity characteristics (amount and spatial distribution). First, using synchrotron x-ray diffraction we show that higher RS in the subsurface region is generated if a lower energy density is used. Second, we show that laser de-focusing and sample positioning inside the build chamber also play an eminent role, and we quantify this influence. In parallel, using X-ray Computed Tomography, we observe that porosity is mainly concentrated in the contour region, except in the case where the laser speed is small. The low values of porosity (less than 1%) do not influence RS.
Neutron diffraction: the forgotten non-destructive technique for residual stress analysis … and more
(2016)
3-D Stress Analysis
(Bulk) Stress mapping
Thick (and thin) films & Interfaces
Bulk high temperature
Real time
In-situ testing: Large sample environment (Stress rigs, Furnaces, …)
Neutrons and Synchrotron Radiation allow all this because they are FASTER , DEEPER and MORE PRECISE than lab equipment
(Flux)(Energy)(Parallel Beam)
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.
Microstructure-property connections for porous ceramics: The possibilities offered by micromechanics
(2016)
Microstructure of porous ceramics is highly “irregular”: it comprises pores and microcracks of diverse shapes and orientations.
This makes their quantitative modeling challenging, and one
often resorts to empirical relations containing Fitting Parameters and having somewhat uncertain range of applicability. We review the substantial progress made in modeling of “irregular” microstructures that does not seem to have been sufficiently utilized in the context of ceramics. We discuss the possibilities offered by micromechanics in developing microstructure–property relations for porous microcracked ceramics. After an overview of relevant micromechanics topics, we focus on several issues of specific interest for ceramics: nonlinear stress–strain behavior, effective elastic properties, and thermally induced microcracking. We discuss extraction of microscale Parameters (such as strength of the intergranular cohesion, density of cracks and pores, etc.) from macroscopic data and identify the extent of uncertainty in this process. We also argue that there is no quantitative correlation between fracturing process and the loss of elastic stiffness.
This study addressed a 7017 Al-alloy tailored for powder bed fusion – laser beam (PBF-LB) process. The alloy was prepared by mixing 3 wt% Zr and 0.5 wt% TiC powder to standard pre-alloyed 7017 grade aluminium powder. This made printing of the alloys possible avoiding solidification cracking in the bulk and achieving high relative density (99.8 %). Such advanced alloys have significantly higher Young’s modulus (>80 GPa) than conventional Al-alloys (70–75 GPa), thus making them attractive for applications requiring high stiffness. The resulting microstructure in as-printed condition was rich in particles originating from admixed powders and primary precipitates/inclusions originating from the PBF-LB process. After performing a T6-like heat treatment designed for the PBF-LB process, the microstructure changed: Zr-nanoparticles and Fe- or Mg/Zn- containing precipitates formed thus providing 75 % increase in yield strength (from 254 MPa to 444 MPa) at the cost of decreasing ductility (∼20 % to ∼9 %). In-situ tensile testing combined with SXCT, and ex-situ tensile testing combined with fracture analysis confirmed that the fracture initiation in both conditions is highly dependent on defects originated during printing. However, cracks are deflected from decohesion around Zr-containing inclusions/precipitates embedded in the Al-matrix. This deflection is seen to improve the ductility of the material.
3D imaging techniques are very fashionable nowadays, and allow enormous progress in understanding ceramic microstructure, its evolution, and its link to mechanical, thermal, and transport properties. In this feature article, we report the use of a powerful, yet not so wide-spread, set of X-ray techniques based on refraction effects. X-ray refraction allows determining internal specific surface (surface per unit volume) in a non-destructive fashion, position and orientation sensitive, and with a nanometric detectability. While the techniques are limited by the X-ray absorption of the material under investigation, we demonstrate showcases of ceramics and composite materials, where understanding of process parameter influence or simply of microstructural parameters could be achieved in a way unrivalled even by high-resolution techniques such as electron microscopy or computed tomography.
Microstructure characterisation of advanced materials via 2D and 3D X-ray refraction techniques
(2018)
3D imaging techniques have an enormous potential to understand the microstructure, its evolution, and its link to mechanical, thermal, and transport properties. In this conference paper we report the use of a powerful, yet not so wide-spread, set of X-ray techniques based on refraction effects. X-ray refraction allows determining internal specific surface (surface per unit volume) in a non-destructive fashion, position and orientation sensitive, and with a nanometric detectability. We demonstrate showcases of ceramics and composite materials, where microstructural parameters could be achieved in a way unrivalled even by high-resolution techniques such as electron microscopy or computed tomography. We present in situ analysis of the damage evolution in an Al/Al2O3 metal matrix composite during tensile load and the identification of void formation (different kinds of defects, particularly unsintered powder hidden in pores, and small inhomogeneity’s like cracks) in Ti64 parts produced by selective laser melting using synchrotron X-ray refraction radiography and tomography.
The microstructure of an apatite-wollastonite (code name AP40) glass-ceramic is analyzed in this study by combining 2D microscopy, phase analysis, X-ray absorption and synchrotron X-ray refraction computed tomography (XCT and SXRCT, respectively). It is shown that this combination provides a useful toolbox to characterize the global microstructure in a wide scale range, from sub-micrometer to millimeter. The material displays a complex microstructure comprising a glassy matrix with embedded fluorapatite and wollastonite small crystals. In this matrix, large (up to 200 μm) spike-shaped structures are distributed. Such microstructural features are oriented around a central sphere, thereby forming a structure resembling a sea urchin. A unique feature of SXRCT, in contrast to XCT, is that internal interfaces are visualized; this allows one to show the 3D distribution of these urchins with exceptionally good contrast. Furthermore, it is revealed that the spike-shaped structures are not single crystals, but rather composed of sub-micrometric crystals, which are identified as fluorapatite and diopside phases by SEM-EDX analysis.
In this Seminar cycle I will present first diffraction methods to determine residual stress and investigate micromechanical properties of complex materials, and then particularize the treatment with applications to porous microcracked ceramics for diesel particulate filter applications.
I will show that neutron diffraction is particularly suited for bulk studies, where 3D stresses are needed. The advantages to use Time-of-Flight or steady state sources will be discussed, together with the problematic of the determination of absolute RS values.
Finally, the behavior of DPF materials under applied load or at high temperatures will be discussed under the combination of macroscopic and microscopic tests.
In this Seminar cycle I will present first diffraction methods to determine residual stress and investigate micromechanical properties of complex materials, and then particularize the treatment with applications to porous microcracked ceramics for diesel particulate filter applications.
I will show that neutron diffraction is particularly suited for bulk studies, where 3D stresses are needed. The advantages to use Time-of-Flight or steady state sources will be discussed, together with the problematic of the determination of absolute RS values.
Finally, the behavior of DPF materials under applied load or at high temperatures will be discussed under the combination of macroscopic and microscopic tests.
We discuss the non-linear stress–strain behavior of microcracked polycrystalline ceramics under uniaxial tension and compression (displacement control).
Micromechanics explanation and modeling of its basic features, such as non-linearity and hysteresis in stress–strain curves, are developed, with stable microcrack propagation and “roughness” of intergranular cracks playing critical roles in tension and crack sliding playing a critical role in compression. Experiments involving complex loading histories are explained, and themodel is shown to reproduce the basic features of the observed stress–strain curves.
The stress-strain behavior of microcracked polycrystalline materials (such as ceramics or rocks) underconditions of tensile, displacement-controlled, loading is discussed. Micromechanical explanation andmodeling of the basic features, such as non-linearity and hysteresis in stress-strain curves, is developed,with stable microcrack propagation and “roughness” of intergranular cracks playing critical roles. Ex-periments involving complex loading histories were done on large- and medium grain sizeb-eucryptiteceramic. The model is shown to reproduce the basic features of the observed stress-strain curves.
The micromechanical behavior of an annealed Ti-6Al-4V material produced by Laser Powder Bed Fusion was characterized by means of in-situ synchrotron X-ray diffraction during a tensile test. The lattice strain evolution was obtained parallel and transversal to the loading direction. The elastic constants were determined and compared with the conventionally manufactured alloy. In the plastic regime, a lower plastic anisotropy exhibited by the lattice planes was observed along the load axis (parallel to the building direction) than in the transverse direction.
Also, the load transfer from α to β phase was observed, increasing global ductility of the material. The material seems to accumulate a significant amount of intergranular strain in the transverse direction.
In this seminar I present the microstructure and micromechanical properties of diesel particulate filter materials, and then particularize them to porous microcracked aluminum titanate.
I show that neutron diffraction is particularly suited for bulk studies, especially under applied load or at high temperatures. The combination of macroscopic and microscopic tests with modeling and simulation yields great added value to understand the mechanics of microcracking.
The paper focuses on the reformulation of classic Maxwell's (1873) homogenization method for calculation of the residual stresses in matrix composites. For this goal, we equate the far fields produced by a set of inhomogeneities subjected to known eigenstrains and by a fictitious domain with unknown eigenstrain. The effect of interaction between the inhomogeneities is reduced to the calculation of the additional field acting on an inhomogeneity due to the eigenstrains in its neighbors. An explicit formula for residual stresses is derived for the general case of a multiphase composite. The method is illustrated by several examples. The results are compared with available experimental data as well as with predictions provided by the non-interaction approximation (Eshelby solution). It is shown that accounting for interaction can explain many experimentally observed phenomena and is required for adequate quantitative analytical modeling of the residual stresses in matrix composites.
A new titanium alloy improving the operation of implants additively manufactured and including laterally closed lattice structures is proposed. The new alloy possesses an increased affinity to the bone. The measured bone–interface implant (BII) of less than 10 mm and bone–implant contact (BIC) of 95% demonstrated an excellent osseointegration. Furthermore, since additive manufacturing naturally leads to a high-roughness surface finish, the wettability of the implant is increased. The combination of these factors is pushing ossification beyond its natural limits. In addition, the quality and speed of the ossification and osseointegration in/around laterally closed lattice implants open the possibility of bone spline key of prostheses. This enables the stabilization of the implant into the bone while keeping the possibility of punctual hooks allowing the implant to be removed more easily if required.
This study examines the relationship between the magnetic mesostructure with the microstructure of low carbon steel tungsten inert gas welds. Optical microscopy revealed variation in the microstructure of the parent material, in the heat affected and fusion zones, correlating with distinctive changes in the local magnetic stray fields measured with high spatial resolution giant magneto resistance sensors. In the vicinity of the heat affected zone high residual stresses were found using neutron diffraction.
Notably, the gradients of von Mises stress and triaxial magnetic stray field modulus follow the same tendency transverse to the weld. In contrast, micro-X-ray fluorescence characterization indicated that local changes in element composition had no independent effect on magnetic stray fields.
Influence of deposition hatch length on residual stress in selective laser melted Inconel 718
(2018)
The present study aims to evaluate the bulk residual stresses in SLM parts by using neutron diffraction measurements performed at E3 line -BER II neutron reactor- of Helmholtz-Zentrum für Materialien und Energie (HZB) Berlin. Together with microstructure characterization and distortion measurements, it is possible to describe the stress state throughout the whole sample. The sample was measured in as-build condition (on a build plate) and after releasing from the build plate. The used material is the nickel based superalloy 718. This alloy is widely used in aerospace and chemical industries due to its superior corrosion and heat resistant properties.
Obtained results indicated different residual stress states for each of the transversal, longitudinal and normal component. The normal and transversal component exhibits a rather compressive behavior while the longitudinal was tensile in the center part of the sample and became compressive towards the tip. As expected, the absolute values of all stress components decreased after releasing the sample from the building plate. A surface scan utilizing a coordinate-measuring machine (CMM) allowed us to present top surface distortion before and after releasing. The top surface showed a distortion around ±80µm after releasing. Microstructure evolution in the scanning-building cross-section is largely dominated by columnar grains. In addition, many small random orientated grains are prominent in the regions of a laser overlap during SLM.
In summary, for the sample of superalloy 718 manufactured by SLM, a small distortion occurred when removing the sample from the build plate whereby the residual stress state decreases. Moreover, the observed columnar grains in the building direction could give a reason for the lowest stress values in that normal direction. However, the most important parameter controlling the residual stresses is the temperature gradient. Hence, future investigations are planned for a different scan strategy to distribute the laser impact in a more homogenous manner.
Influence of a 265 °C heat treatment on the residual stress state of a PBF-LB/M AlSi10Mg alloy
(2022)
Laser Powder Bed Fusion (PBF-LB/M) additive manufacturing (AM) induces
high magnitude residual stress (RS) in structures due to the extremely heterogeneous cooling and heating rates. As the RS can be deleterious to the fatigue resistance of engineering components, great efforts are focused on understanding their generation and evolution after post-process heat treatments. In this study, one of the few of its kind, the RS relaxation induced in an as-built PBF-LB/M AlSi10Mg material by a low-temperature heat treatment (265 °C for 1 h) is studied by means of X-ray and neutron diffraction. Since the specimens are manufactured using a baseplate heated up to 200 °C, low RS are found in the as-built condition. After heat treatment a redistribution of the RS is observed, while their magnitude remains constant. It is proposed that the redistribution is induced by a repartition of stresses between the a-aluminium matrix and the silicon phase, as the morphology of the silicon phase is affected by the heat treatment. A considerable scatter is observed in the neutron diffraction RS profiles, which is principally correlated to the presence (or absence) of pockets of porosity developed at the borders of the chessboard pattern.
The porosity and the surface roughness are recently discussed problems for SLM parts. The influence of SLM process parameters on porosity is well studied for different materials. Nevertheless, the build angle (i.e. the angle between part orientation and build plate) needs to be understood as an additional SLM process parameter, as it has been shown, that the microstructure and hence the mechanical performance of various materials depend on the build angle. The inherent build angle of each strut as a part of a lattice structure is the motivation to investigate the influence of the build angle on the porosity and roughness on round-shaped (1 mm diameter) struts by means of CT. Conventional Coordinate Measuring Machine (CMM) has the limitation towards small and round shaped samples. The need for Computed Tomography (CT) regarding investigations of SLM parts will increase because no other non-destructive technique allows the assessment of complex geometries with inner laying surfaces. We used CT to assess the pores and the strut surface. Seven struts out of the nickel alloy Inconel 625 with build angles from 30° to 90° were studied. It was found that the number of pores is smaller, and the size of pores is larger for the 90° strut. In case of 30° strut, the number of pores is increased towards down-skin side, additionally, this strut orientation showed to have the largest number of attached powder particles. The elongated pores exist exclusively near the strut surface. While the roughness at the down-skin surface is highly depending of the biud angle, the roughness at the up-skin surface is the same for all struts. The mechanisms of pore and surface roughness formation is not mainly driven by gravity.
Several cylindrical specimens and dental implants, presenting diagonal lattice structures with different cell sizes (600, 900 and 1200 µm) were additively manufactured by selective laser melting process. Then they were implanted for two months in a sheep. After removal, they were studied by Archimedes’ method as well as X-ray computed tomography in order to assess the penetration of bone into the lattice. We observed that the additive manufactured parts were geometrically conform to the theoretical specifications. However, several particles were left adhering to the surface of the lattice, thereby partly or entirely obstructing the cells. Nevertheless, bone penetration was clearly visible. We conclude that the 900 µm lattice cell size is more favourable to bone penetration than the 1200 µm lattice cell size, as the bone penetration is 84 % for 900 µm against 54 % for 1200 µm cell structures. The lower bone penetration value for the 1200 µm lattice cell could possibly be attributed to the short residence time in the sheep. Our results lead to the conclusion that lattice implants additively manufactured by selective laser melting enable better bone integration.
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.
The in situ analysis of the damage evolution in a metal Matrix composite (MMC) using synchrotron X-ray refraction radiography (SXRR) is presented. The investigated material is an Al alloy (6061)/10 vol% Al2O3 MMC after T6 heat treatment.
In an interrupted tensile test the gauge section of dog bone-shaped specimens is imaged in different states of tensile loading. On the basis of the SXRR images, the relative change of the specific surface (proportional to the amount of damage) in the course of tensile loading was analyzed. It could be shown that the damage can be detected by SXRR already at a stage of tensile loading, in which no Observation of damage is possible with radiographic absorption-based imaging methods.
Moreover, the quantitative analysis of the SXRR images reveals that the amount of damage increases homogeneously by an average of 25% with respect to the Initial state. To corroborate the experimental findings, the damage distribution was imaged in 3D after the final tensile loading by synchrotron X-ray refraction computed tomography (SXRCT) and absorption-based synchrotron X-ray computed tomography (SXCT). It could be evidenced that defects and damages cause pronounced indications in the SXRCT images.
Talbot-Lau interferometry provides X-ray imaging techniques with significant enhancement of the radiographic contrast of weakly absorbing objects. The grating based technique allows separation of absorption, refraction and small angle scattering effects. The different efficiency of rectangular and triangular shaped phase gratings at varying detector distances is investigated. The interference patterns (Talbot carpets) are modeled for parallel monochromatic radiation and measured by synchrotron radiation. In comparison to rectangular shapes of phase gratings much higher visibility is obtained for triangular shapes which yield enhanced contrast of a glass capillary test specimen.
Contour scanning and process gas type are process parameters typically considered achieving second order effects compared to first order factors such as laser power and scanning speed. The present work highlights that contour scanning is crucial to ensure geometrical accuracy and thereby the high performance under uniaxial compression of complex Alloy 718 lattice structures. Studies of X-ray computed tomography visualizations of as-built and compression-strained structures reveal the continuous and smooth bending and compression of the walls, and the earlier onset of internal contact appearance in the denser lattices printed with contour. In contrast, the effect of addition of He to the Ar process gas appears to have limited influence on the mechanical response of the lattices and their microstructure as characterized by electron backscattered diffraction. However, the addition of He proved to significantly enhance the cooling rate and to reduce the amount of the generated spatters as evidenced by in situ monitoring of the process emissions, which is very promising for the process stability and powder reusability during laser powder bed fusion.
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.
The present work offers an explanation for the variation of the power-law stress exponent, n, with the stress r normalized to the shear modulus G in aluminum alloys. The approach is based on the assumption that the dislocation structure generated with deformation has a fractal nature. It fully explains the evolution of n with r/G even beyond the so-called power law breakdown region. Creep data from commercially pure Al99.8%, Al-3.85%Mg, and ingot AA6061 alloy tested at different temperatures and stresses are used to validate the proposed ideas. Finally, it is also shown that the fractal description of the dislocation structure agrees well with current knowledge.
Powder Bed Fusion – Laser Beam (PBF-LB) of high γ’ strengthened Ni-base superalloys, such as CM247LC, is of great interest for high temperature applications in gas turbines. However, PBF-LB of CM247LC is challenging due to the high cracking susceptibility during PBF-LB processing (solidification cracking) and heat treatment (strain age cracking, mostly caused by residual stresses). This study focuses on understanding the impact of process parameters on microstructure, residual stresses and solidification cracking. Laser power (P), speed (v) and hatch spacing (h) were varied while the layer thickness (t) was fixed. The melt pool size and shape were found to be key factors in minimizing solidification cracking. Narrower and shallower melt pools, achieved using a low line energy density (LED = P/v ≤ 0.1 J/mm), gave low crack densities (0.7 mm/mm2). A tight hatch spacing (h = 0.03 mm) resulted in reduced lack of fusion porosity. Electron backscatter diffraction investigations revealed that parameters giving finer microstructure with 〈100〉crystallographic texture had low crack densities provided they were processed with a low LED. Atom probe tomography elucidated early stages of spinodal decomposition in the as-built condition, where Cr and Al cluster separately. The extent of spinodal decomposition was found to be affected by the LED and the hatch spacing. Samples with low LED and small hatch spacing showed higher degrees of spinodal decomposition. X-ray diffraction residual stress investigations revealed that the residual stress is proportional to the volumetric energy density (VED = P/(v. h. t)). Although low residual stresses can be achieved by using low VED, there is a high risk of lack of fusion. Hence, other parameters such as modified scan strategy, build plate pre-heating and pulsed laser mode, must be further explored to minimize the residual stresses to reduce the strain age cracking susceptibility.
The availability of high-performance Al alloys in AM is limited due to difficulties in printability, requiring both the development of synergetic material and AM process to mitigate problems such as solidification cracking during laser powder bed fusion (LPBF). The goal of this work was to investigate the failure mechanism in a LPBF 7017 Aluminium alloy + 3 wt% Zr + 0.5 wt% TiC. The processing leads to different categories of Zr-rich inclusions, precipitates and defects.
Subsurface residual stresses (RS) were investigated in Ti-6Al-4V cuboid samples by means of X-ray synchrotron diffraction. The samples were manufactured by laser powder bed fusion (LPBF) applying different processing parameters, not commonly considered in open literature, in order to assess their influence on RS state. While investigating the effect of process parameters used for the calculation of volumetric energy density (such as laser velocity, laser power and hatch distance), we observed that an increase of energy density led to a decrease of RS, although not to the same extent for every parameter variation. Additionally, the effect of support structure, sample roughness and LPBF machine effects potentially coming from Ar flow were studied. We observed no influence of support structure on subsurface RS while the orientation with respect to Ar flow showed to have an impact on RS.We conclude recommending monitoring such parameters to improve part reliability and reproducibility.
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.