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Paper des Monats
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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.
Additive Manufacturing by Selective Laser Melting (SLM) offers an ample scope for producing geometrically complex parts as compared to the traditional subtractive manufacturing strategies. However, the residual stresses (RS) developed during the processing can reduce the load bearing capacity as well as induce unwanted distortion, limiting the life time and the application of SLM parts.
With the recent rise in the demand for additive manufacturing (AM), the need for reliable simulation tools to support experimental efforts grows steadily. Computational welding mechanics approaches can simulate the AM processes but are generally not validated for AM-specific effects originating from multiple heating and cooling cycles. To increase confidence in the outcomes and to use numerical simulation reliably, the result quality Needs to be validated against experiments for in-situ and post-process cases. In this article, a validation is demonstrated
for a structural thermomechanical simulation model on an arbitrarily curved Directed Energy Deposition (DED)part: at first, the validity of the heat input is ensured and subsequently, the model’s predictive quality for in-situ
deformation and the bulging behaviour is investigated. For the in-situ deformations, 3D-Digital Image Correlation measurements are conducted that quantify periodic expansion and shrinkage as they occur. The results show a strong dependency of the local stiffness of the surrounding geometry. The numerical Simulation model is set up in accordance with the experiment and can reproduce the measured 3-dimensional in-situ displacements. Furthermore, the deformations due to removal from the substrate are quantified via 3D-scanning, exhibiting considerable distortions due to stress relaxation. Finally, the prediction of the deformed shape is discussed in regards to bulging simulation: to improve the accuracy of the calculated final shape, a novel Extension of the model relying on the modified stiffness of inactive upper layers is proposed and the experimentally observed bulging could be reproduced in the finite element model.
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.
Additive manufacturing (AM) offers an effective solution to the medical sector. It enables the production, on demand, of customised implants which match the patient’s anatomy, with grafts that promote bone growth, as well as surgical guides that help the surgeons.
The objective of this project is to provide a comprehensive basis to enable the safe use of medical AM products with traceable and reliable dimensionalmeasurements. This will guarantee the reliability of medical AM products to notified bodies and facilitate acceptance of AM in the medical sector for a better quality of life.
Glass-ceramics are noted for their unusual combination of properties and manifold commercialized products for consumer and specialized markets. Evolution of novel glass and ceramic processing routes, a plethora of new compositions, and unique exotic nano- and microstructures over the past 60 years led us to review the Definition of glass-ceramics. Well-established and emerging processing methods, such as co-firing, additive manufacturing, and laser patterning are analyzed concerning the core requirements of processing glass-ceramics and the Performance of the final products. In this communication, we propose a revised, updated definition of glass-ceramics, which reads “Glass-ceramics are inorganic, non-metallic materials prepared by controlled crystallization of glasses via different processing methods. They contain at least one type of functional crystalline phase and a residual glass. The volume fraction crystallized may vary from ppm to almost 100%”.
Having been introduced almost two decades ago, Additive Manufacturing (AM) of metals has become industrially viable for a large variety of applications, including aerospace, automotive and medicine. Powder bed techniques such as Selective Laser Melting (SLM) based on layer-by-layer deposition and laser melt enable numerous degrees of freedom for the geometrical design. Developing during the manufacturing process, residual stresses may limit the application of SLM parts by reducing the load bearing capacity as well as induce unwanted distortion depending on the boundary conditions specified in manufacturing.
The residual stress distribution in IN718 elongated prisms produced by SLM was studied non-destructively by means of neutron (bulk) and laboratory X-ray (surface) diffraction. The samples with different scanning strategies, i.e. hatching length, were measured in as-built condition (on a build plate) and after removal from the build plate.
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.
Together with surface scan utilizing a coordinate-measuring machine (CMM), it is possible to link the stress release to the sample distortion.
We finally propose an explanation of those stress profiles based on the deposition strategy.
We investigated lattice structure manufactured by laser beam melting with computed tomography on difference scales, such as powder scale, strut scale and lattice scale.
The raw powder has been evaluated by means of synchrotron computed tomography (CT) at the BAM-Line (HZB Bessy II, Berlin). Therefore, the particle size distribution and even the pore size distribution was investigated and compared with results received by the producer by means of sieving. Studies with laboratory X-ray CT of porosity and roughness of manufactured struts in dependence of the build angle exhibited the tendency that elongated pores appear solely in a certain range near the edge. The integrity and load-bearing capacity of a lattice structure was investigated by means of in-situ CT during compression. The lattice structure was compressed by 10 % in height with an applied maximum force of 5 kN. We applied digital volume correlation algorithm on volumes of different load steps to quantifies the displacement within the structure.
Im Fokus dieser Arbeit steht die computertomographische (CT) Untersuchung (Synchrotron- und Labor-CT) von IN625-Pulver und den daraus gefertigten Streben, welche wiederum zu Gitterstrukturen zusammengesetzt werden. Aufgrund der Filigranität wurde zur Fertigung dieser Proben das pulverbettbasierte selektive Laserschmelzen verwendet.
Porositätsanalysen und Größenverteilungen wurden für das Pulver bei einer rekonstruierten Voxelgröße von 0,5µm ermittelt. 6,0mm lange Streben variierten im Aufbauwinkel von 30° bis 90° zur Bauplattform und zeigten so den Unterschied zwischen Up- und Down-Skin hinsichtlich der Rauigkeit und Porenverteilung. Die Gitterstrukturen konnten in-situ mit bis zu 5,0kN belastet werden, um deren Verformung computertomographisch zu erfassen.
The topic of the presentation consists in some basic considerations on the application of fracture mechanics to fatigue live and strengh prediction of metallic componends manufatured by additive manufacturing. These are based on an approach developed at BAM which comprises elements such as the elastic-plastic modelling of the cyclic crack driving force, a physically meaningfull determination of the initial crack size and multipile crack initiation and propagation due to variations of the local geometry and material charactaristics. Spezial emphasis is put to spezific aspects of materials composed by selectiv laser melting such as surface roughness, porosity and gradiants in the microstructure.
Powder bed -based technologies are amongst the most successful Additive Manufacturing (AM) techniques. "Selective laser sintering/melting" (SLS/SLM) and "binder jetting 3D printing" (3DP) especially are leading AM technologies for metals and polymers, thanks to their high productivity and scalability. In this context, the "layerwise slurry deposition" (LSD) has been developed as a layer deposition method which enables the use of SLS/SLM and 3DP technologies for advanced ceramic materials. LSD consists in the layer-by-layer deposition of a ceramic slurry by means of a doctor blade. Each layer is deposited and dried to achieve a highly packed powder layer, which can be used for SLM or for 3DP. This technique offers high flexibility in the ceramic feedstock used, especially concerning material and particle size, and is capable of producing parts with physical and mechanical properties comparable to traditionally shaped parts. In this presentation, the LSD technique will be introduced and several examples of application to porcelain, SiC and alumina products will be reported.
In powder-based Additive Manufacturing (AM) processes, an object is produced by successively depositing thin layers of a powder material and by inscribing the cross section of the object in each layer. The main methods to inscribe a layer are by binder jetting (also known as powder 3D printing) or by selective laser sintering/melting (SLS/SLM).
Powder-based AM processes have found wide application for several metallic, polymeric and also ceramic materials, due to their advantages in combining flexibility, easy upscaling and (often) good material properties of their products.
The deposition of homogeneous layers is key to the reproducibility of these processes and has a direct influence on the quality of the final parts. Accordingly, powder properties such as particle size distribution, shape, roughness and process related properties such as powder flowability and packing density need to be carefully evaluated.
Due to these requirements, these processes have been so far precluded to find commercial use for certain applications. In the following, two outstanding cases will be presented.
A first example is that powder-based AM processes are widely used for many metallic and polymeric materials, but they find no commercial application for most technical ceramics.
This seemingly contradicting observation is explained by the fact that in powder based AM, a dry flowable powder needs to be used. The processing of technical ceramics in fact typically requires very fine and poorly flowable powder, which makes them not suitable for the standard processes. There have been several approaches to adapt the raw materials to the process (e.g. by granulation), but in order to maintain the superior properties of technical ceramics it seems necessary to follow the opposite approach and adapt the process to the raw materials instead.
This was the motivation for developing the Layerwise Slurry Deposition (LSD), an innovative process for the deposition of powder layers with a high packing density. In the LSD process, a ceramic slurry is deposited to form thin powder layers, rather than using a dry powder. This allows achieving high packing density (55-60%) in the layers after drying. It is also important, that standard ceramic raw materials can be used. When coupled with a printing head or with a laser source, the LSD enables novel AM technologies which are similar to 3D printing or selective laser sintering, but taking advantage of having a highly dense powder bed.
The LSD -3D printing, in particular, offers the potential of producing large (> 100 mm) and high quality ceramic parts, with microstructure and properties similar to traditional processing. Moreover, due to the compact powder bed, no support structures are required for fixation of the part in the printing process.
Figure 1 shows the schematics of the working principle of the LSD-3D print and illustrates some examples of the resolution and features achievable.
The second outstanding case here described is the application of powder-based AM in environments with reduced or zero gravity. The vision is to be able to produce repair parts, tools and other objects during a space mission, such as on the International Space Station (ISS), without the need of delivering such parts from Earth or carrying them during the mission. AM technologies are also envisioned to play an important role even for future missions to bring mankind to colonize other planets, be it on Mars or on the Moon. In this situation, reduced gravity is also experienced (the gravitational acceleration is 0.16 g on the Moon and 0.38 g on Mars).
These environments cause the use of AM powder technologies to be very problematic: the powder layers need to be stabilized in order to avoid dispersion of the particles in the chamber. This is impossible for standard AM powder deposition systems, which rely on gravitation to spread the powder.
Also in this case, an innovative approach has been implemented to face this technological challenge. The application of a gas flow through a powder has a very strong effect on its flowability, by generating a force on each particle, which is following the gas flow field. This principle can be applied in a simple setup such as the one shown in Figure 2.
In this setup, the gas flow causes an average pressure on the powder bed in direction of the arrows, generating a stabilizing effect which acts in the same direction of the gravitational force. This effect can be used in addition to normal gravity on Earth to achieve a better stabilization of 3D printed parts in the powder bed. In this case, even a significant increase of packing density of the powder was measured, compared to the same experimental setup without gas flow. This is due to the fact that the force on each single particle follows the gas flow field, which is guiding the particles to settle between the pores of the powder bed, thus achieving an efficient packing.
The same principle can be applied in absence of gravitation, where the gas flow acts to stabilize the powder layers. It has been shown that ceramic powder could be deposited in layers and laser sintered in µ-gravity conditions during a DLR (Deutsches Zentrum für Luft- und Raumfahrt) campaign of parabolic flights, as shown in Figure 2. A follow-up campaign is dedicated to the deposition of metallic (stainless steel) powder in inert atmosphere and to study the effects of laser melting in µ-gravity.
In conclusion, the description of these two example cases shows how the development of novel technological processes can address some of the limitations of standard powder-based AM, in order to enable the use of new materials, such as technical ceramics, or to tackle the challenges of AM in space.
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 synchrotron- and 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 a dependence of the residual state on the penetration depth in the sample. For the surface residual stresses, longitudinal and transverse stress components from both 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.
Virtual-lab-based determination of a macroscopic yield function for additively manufactured parts
(2018)
This work presents a method for the yield function determination of additively manufactured parts of S316L steel. A crystal plasticity model is calibrated with test results and used afterwards to perform so-called virtual experiments, that account for the specific process-related microstructure including crystallographic and morphological textures. These simulations are undertaken on a representative volume element (RVE), that is generated from EBSD/CT-Scans on in-house additively manufactured specimen, considering grain structure and crystal orientations. The results of the virtual experiments are used to determine an anisotropic Barlat yield function, that can be used in a macroscopical continuum-sense afterwards. This scale-bridging approach enables the calculation of large-scale parts, that would be numerically too expensive to be simulated by a crystal plasticity model.
The quality of components made by laser beam melting (LBM) additive manufacturing is naturally influenced by the quality of the powder bed. A packing density < 1 and porosity inside the powder particles lead to intrinsic voids in the powder bed. Since the packing density is determined by the particle size and shape distribution, the determination of these properties is of significant interest to assess the printing process. In this work, the size and shape distribution, the amount of particle’s intrinsic porosity as well as the packing density of micrometric powder used for LBM have been investigated by means of synchrotron X-ray computed tomography (CT). Two different powder batches were investigated: Ti-6Al-4V produced by plasma atomization and Stainless Steel 316L produced by gas atomization. Plasma atomization particles were observed to be more spherical in terms of the mean anisotropy compared to particles produced by gas atomization. The two kinds of particles are comparable in size according to the equivalent diameter. The packing density is lower (i.e. the powder bed contains more voids in between particles) for the Ti-6Al-4V particles. The comparison of the tomographic results with laser diffraction, as another particle size measurements techniques, proved agreement.
Most additive manufacturing processes which produce dense ceramics are nowadays limited in size because of inevitable post-processing steps like for example binder removal in stereolithography. The additive manufacturing of voluminous ceramic parts is realized by powder bed based processes which, however, generate parts with residual porosity. Via infiltration these parts can be processed to dense parts like for example SiC but this is not possible for all ceramics like for example Si3N4. There is a lack of methods for the additive manufacturing of dense voluminous parts for most ceramics.
We have developed a new additive manufacturing technology, the Laser Induced Slip casting (LIS), based on the layerwise deposition of slurries and their local drying by laser radiation. Laser Induced Slip casting generates ceramic green bodies which can be sintered to dense ceramic components like traditional formed ceramic powder compacts. We will introduce the LIS technology, green bodies and sintered parts will be shown and their microstructure and mechanical properties will be discussed.
Most additive manufacturing processes which produce dense ceramics are nowadays limited in size because of inevitable post-processing steps like for example binder removal in stereolithography. The additive manufacturing of voluminous ceramic parts is realized by powder bed based processes which, however, generate parts with residual porosity. Via infiltration these parts can be processed to dense parts like for example SiC but this is not possible for all ceramics like for example Si3N4. There is a lack of methods for the additive manufacturing of dense voluminous parts for most ceramics.
We have developed a new additive manufacturing technology, the Laser Induced Slip casting (LIS), based on the layerwise deposition of slurries and their local drying by laser radiation. Laser Induced Slip casting generates ceramic green bodies which can be sintered to dense ceramic components like traditional formed ceramic powder compacts. We will introduce the LIS technology, green bodies and sintered parts will be shown and their microstructure and mechanical properties will be discussed.
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.