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Eingeladener Vortrag
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For the first time, X-ray refraction techniques are proven for the identification of void formation in Ti-6Al-4V parts produced by selective laser melting. The topology and volume fraction of pores are measured in samples produced with different laser energy density. Unique X-ray refraction methods identify different kinds of defects, characteristic to the regions below and above the Optimum laser energy density, namely unprocessed powder (unmolten powder particles, balling effect, and Fusion defects) from empty keyhole pores. Furthermore, it is possible to detect small inhomogeneities (voids or cracks) with sizes below the spatial resolution of optical microscopy and X-ray computed tomography.
Functional materials for energy conversion are important technology drivers needed for the implementation of low carbon energy. Therefore, researchers commonly focus on improving the intrinsic properties of a functional material. However, for applications, the extrinsic properties are at least as important as the intrinsic ones. Consequently, it is important to investigate and understand the external and internal structure of semi-finished products and especially defect dependent properties. The extrinsic properties may change during application and the life cycle of the material as well as through processing and molding steps.
Our studies show how X-ray tomographic (XCT) investigations can contribute to structure investigations in composites and massive samples using the example of magnetic materials for energy conversion. The components are tested non-destructively in 3D in order to localize and characterize cracks, pores, inclusions as well as other defects and their influence on the functional properties and also “in-time” during the life cycle of the material. Exsitu and in-situ experiments performed with non-destructive XCT are predestinated to follow damaging mechanisms of materials under certain load conditions, atmospheres or liquids, e.g. went through several working cycles of a functional material. By combining microtomography with other methods of magnetic and classical material characterization, unique statements about the structure and the functional properties can be made.
From the applications point of view, sometimes complex, three-dimensional geometries are needed to fully exploit the functional properties of the materials, e.g. to ensure a high surface area for heat exchange. Since many functional materials are brittle and difficult to form, shaping is often a big challenge. In principle, additive manufacturing processes offer the possibility to produce complex, porous components from poorly formable alloys.
If all stages of additive manufacturing are accompanied by X-ray tomographic imaging, the process of finding the optimal parameters for material processing can be significantly accelerated.
Based on the quality control of the initial powder material used and also investigations of the shape and arrangement of defects within the molten structure and their relationship with the melting path scanning strategy, Xray tomography has proven to be an ideal tool for additive manufacturing, even for functional materials. Overall, tomographic methods are important tools for the development of functional materials to application maturity.
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.
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.
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.
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.
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 effect of two types of scanning strategies on the grain structure and build-up of Residual Stress (RS) has been investigated in an as-built IN718 alloy produced by Laser Powder Bed Fusion (LPBF). The RS state has been investigated by X-ray diffraction techniques. The microstructural characterization was performed principally by Electron Backscatter Diffraction (EBSD), where the application of a post-measurement refinement technique enables small misorientations (< 2°) to be resolved. Kernel average misorientation (KAM) distributions indicate that preferably oriented columnar grains contain higher levels of misorientation, when compared to elongated grains with lower texture. The KAM distributions combined with X-ray diffraction stress maps infer that the increased misorientation is induced via plastic deformation driven by the thermal stresses, acting to self-relieve stress. The possibility of obtaining lower RS states in the build direction as a consequence of the influence of the microstructure should be considered when envisaging scanning strategies aimed at the mitigation of RS.
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.
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.
Alternative to conventional transmission-based radiography and computed tomography, X-ray refraction techniques are being increasingly used to detect damage in light materials. In fact, their range of application has been recently extended even to metals. The big advantage of X-ray refraction techniques is that they are able to detect nanometric defects, whose size would lie below the resolution of even state-of-the-art synchrotron-based X-ray computed tomography (SXCT). The superiority of synchrotron X-ray refraction radiography and tomography (SXRR and SXRCT) has been shown in the case of light materials, in particular composites. X-ray refraction techniques also yield a quantitifaction of the amount of damage (the so-called relative internal specific surface) and can well be compared with damage models. At the same time, it is impossible for SXRR and SXRCT to image single defects. We show that the combination of refraction- and transmission-based imaging techniques yields an impressive amount of additional information about the type and amount of defects in microstructured materials such as additively manufactured metals or metal matrix composites. We also show that the use of data fusion techniques allows the classification of defects in statistically significant representative volume elements.
Alternative to conventional transmission-based radiography and computed tomography, X-ray refraction techniques are being increasingly used to detect damage in light materials. In fact, their range of application has been recently extended even to metals. The big advantage of X-ray refraction techniques is that they are able to detect nanometric defects, whose size would lie below the resolution of even state-of-the-art synchrotron-based X-ray computed tomography (SXCT). The superiority of synchrotron X-ray refraction radiography and tomography (SXRR and SXRCT) has been shown in the case of light materials, in particular composites. X-ray refraction techniques also yield a quantitifaction of the amount of damage (the so-called relative internal specific surface) and can well be compared with damage models. At the same time, it is impossible for SXRR and SXRCT to image single defects. We show that the combination of refraction- and transmission-based imaging techniques yields an impressive amount of additional information about the type and amount of defects in microstructured materials such as additively manufactured metals or metal matrix composites. We also show that the use of data fusion techniques allows the classification of defects in statistically significant representative volume elements.
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.
This study investigates the room‐ and high‐temperature (650 °C) tensile and low‐cycle‐fatigue behavior of Inconel 718 produced by laser powder bed fusion (PBF‐LB/M) with a four‐step heat treatment and compares the results to the conventional wrought material. The microstructure after heat treatment is characterized on different length scales. Compared to the wrought variant, the elastic and yield properties are comparable at both test temperatures while tensile strength, ductility, and strain hardening capacity are lower. The fatigue life of the PBF‐LB/M variant at room temperature is slightly lower than that of the wrought material, while at 650 °C, it is vice versa. The cyclic stress response for both material variants is characterized by cyclic softening, which is more pronounced at the higher test temperature. High strain amplitudes (≥0.7%) at room temperature and especially a high testing temperature result in the formation of multiple secondary cracks at the transitions of regions comprising predominantly elongated grain morphology and columns of stacked grains with ripple patterns in the PBF‐LB/M material. This observation and pronounced crack branching and deflection indicate that the cracks are controlled by sharp micromechanical gradients and local crystallite clusters.
The complexity of any microstructural characterization significantly increases when there is a need to evaluate the icrostructural evolution as a function of temperature. To date, this characterization is primarily performed by undertaking elaborative ex-situ experiments where the material’s heating procedure is interrupted at different temperatures or times. Moreover, these studies are often limited to a region smaller than the representative elementary volume, which can lead to partial or even biased interpretations of the collected data. This limitation can be greatly overcome by using in-situ synchrotron X-ray refraction (SXRR).
Synchrotron based absorption edge tomography for the analysis of 3D printed polymer embedded MOF
(2019)
Absorption edge tomography, also known as differential tomography at absorption edges, is a method which exploits the sudden change of the attenuation coefficient, when the photon energy crosses the absorption edge of an element. Synchrotron radiation is the best source for absorption edge tomography, because of its small bandwidth, high intensity and easily adjustable photon energy. The synchrotron beamline BAMline at the synchrotron radiation facility BESSY II in Berlin, which is operated by the Bundesanstalt für Materialforschung und -prüfung (BAM), provides a monochromatized beam in a photon energy range from 5 keV up to 80 keV with a bandwidth of 2%, when the double multilayer monochromator is used. Together with the microtomography setup, this enables differential tomography with submicron resolution at the K edge of the elements from chromium up to the lanthanides, and up to uranium, when the L edges are used as well.
In this work, metal organic frameworks (MOFs) embedded in polymer are characterized using differential tomography. MOFs are microporous structures of metal ions, coordinated by organic linker molecules, that can be used in a broad field of applications, especially in gas storage and catalysis. In this work, polymer embedded MOFs were extruded into filaments, which were subsequently used for 3d-printing to profit from the specific properties of the MOFs in polymeric materials combined with the arbitrary shapes provided by 3d-printing. For the extrusion, different polymer classes like ABS, polyester- and polyetherurethanes, as well as different MOFs (ZIF-8, ZIF-67, HKUST-1) were used to create MOF containing filaments with a nominal diameter of 3.0 mm. Differential tomography at the edges of the Zn, Co, and Cu was then used to find the distribution of the corresponding MOF in the filament and to analyze the shape of the inclusions.
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.
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.
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.