Project description:The effect of microstructure on the susceptibility to selective corrosion of Alloy 625 produced by laser powder bed fusion (LPBF) process was investigated through intergranular corrosion tests according to ASTM G28 standard. The effect of heat treatment on selective corrosion susceptibility was also evaluated. The behavior was compared to commercial hot-worked, heat treated Grade 1 Alloy 625. The morphology of attack after boiling ferric sulfate-sulfuric acid test according to ASTM G28 standard is less penetrating for LPBF 625 alloy compared to hot-worked and heat-treated alloy both in as-built condition and after heat treatment. The different attack morphology can be ascribed to the oversaturation of the alloying elements in the nickel austenitic matrix obtained due to the very high cooling rate. On as-built specimens, a shallow selective attack of the border of the melt pools was observed, which disappeared after the heat treatment. The results confirmed similar intergranular corrosion susceptibility, but different corrosion morphologies were detected. The results are discussed in relation to the unique microstructures of LPBF manufactured alloys.
Project description: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.
Project description:A non-equiatomic AlCoCr0.75Cu0.5FeNi alloy has been identified as a potential high strength alloy, whose microstructure and consequently properties can be widely varied. In this research, the phase structure, hardness, and magnetic properties of AlCoCr0.75Cu0.5FeNi alloy fabricated by laser powder bed fusion (LPBF) are investigated. The results demonstrate that laser power, scanning speed, and volumetric energy density (VED) contribute to different aspects in the formation of microstructure thus introducing alterations in the properties. Despite the different input parameters studied, all the as-built specimens exhibit the body-centered cubic (BCC) phase structure, with the homogeneous elemental distribution at the micron scale. A microhardness of up to 604.6 ± 6.8 HV0.05 is achieved owing to the rapidly solidified microstructure. Soft magnetic behavior is determined in all as-printed samples. The saturation magnetization (Ms) is dependent on the degree of spinodal decomposition, i.e., the higher degree of decomposition into A2 and B2 structure results in a larger Ms. The results introduce the possibility to control the degree of spinodal decomposition and thus the degree of magnetization by altering the input parameters of the LPBF process. The disclosed application potentiality of LPBF could benefit the development of new functional materials.
Project description:Shape memory alloys (SMAs) are functional materials that are being applied in practically all industries, from aerospace to biomedical sectors, and at present the scientific and technologic communities are looking to gain the advantages offered by the new processing technologies of additive manufacturing (AM). However, the use of AM to produce functional materials, like SMAs, constitutes a real challenge due to the particularly well controlled microstructure required to exhibit the functional property of shape memory. In the present work, the design of the complete AM processing route, from powder atomization to laser powder bed fusion for AM and hot isostatic pressing (HIP), is approached for Cu-Al-Ni SMAs. The microstructure of the different processing states is characterized in relationship with the processing parameters. The thermal martensitic transformation, responsible for the functional properties, is analyzed in a comparative way for each one of the different processed samples. The present results demonstrate that a final post-processing thermal treatment to control the microstructure is crucial to obtain the expected functional properties. Finally, it is demonstrated that using the designed processing route of laser powder bed fusion followed by a post-processing HIP and a final specific thermal treatment, a satisfactory shape memory behavior can be obtained in Cu-Al-Ni SMAs, paving the road for further applications.
Project description:In-depth understanding of microstructure development is required to fabricate high quality products by additive manufacturing (for example, 3D printing). Here we report the governing role of side-branching in the microstructure development of alloys by laser powder bed fusion. We show that perturbations on the sides of cells (or dendrites) facilitate crystals to change growth direction by side-branching along orthogonal directions in response to changes in local heat flux. While the continuous epitaxial growth is responsible for slender columnar grains confined to the centreline of melt pools, side-branching frequently happening on the sides of melt pools enables crystals to follow drastic changes in thermal gradient across adjacent melt pools, resulting in substantial broadening of grains. The variation of scan pattern can interrupt the vertical columnar microstructure, but promotes both in-layer and out-of-layer side-branching, in particular resulting in the helical growth of microstructure in a chessboard strategy with 67° rotation between layers.
Project description:Microstructures and age-hardening phenomena of directly aged (artificial aged) AlSi10Mg alloys fabricated by laser powder bed fusion (LPBF) were characterized using scanning transmission electron microscopy, atom probe tomography, and Vickers hardness testing. The microstructure derived from overlapping melt pools has a full cellular structure consisting of eutectic Si walls surrounding α-Al cells. In the initial stage of aging, solute clusters with density on the order of 1024/m3 were formed in α-Al cells. By prolonging the aging time further, fine Si particles of about 50 nm in diameter precipitated. Before Si precipitation, the hardness of the aged sample was clearly greater than that of the as-built state. With further aging time, the hardness increased further because of the Si precipitation. Cluster analysis revealed that the number density and the size of clusters increased from as-built state by aging, whereas the types of the solute clusters remained almost unchanged by aging. The results indicate that the nanoscale clusters within the α-Al cells, which increase via aging, produce age-hardening effect.
Project description:The present study introduces an approach to the powder metallurgical shaping of a pseudo-elastic nickel-titanium (NiTi 44 alloy) combining two different Additive Manufacturing (AM) processes, namely fused filament fabrication (FFF) and Laser Powder Bed Fusion (LPBF), by manufacturing filigree structures on top of sintered FFF parts. Both processes start with commercial gas atomized NiTi powder, which is fractionated into two classes. Using the fine fraction with particle sizes <15 µm, robust thermoplastic filaments based on a non-commercial binder system were produced and processed to different auxetic and non-auxetic geometries employing a commercial standard printer. FTIR analysis for thermal decomposition products was used to develop a debinding regime. After sintering, the phase transformation austenite/martensite was characterized by DSC in as sintered and annealed state. Precipitates resulting from residual impurities were detected by micrographs and XRD. They led to an increased transformation temperature. Adjusting the oxygen and carbon content in the alloy remains a challenging issue for powder metallurgical processed NiTi alloys. Filigree lattice structures were built onto the surfaces of the sintered FFF parts by LPBF using the coarser powder fraction (15-45 µm). A good material bond was formed, resulting in the first known NiTi hybrid, which introduces new production and design options for future applications.
Project description:High-throughput experiments that use combinatorial samples with rapid measurements can be used to provide process-structure-property information at reduced time, cost, and effort. Developing these tools and methods is essential in additive manufacturing where new process-structure-property information is required on a frequent basis as advances are made in feedstock materials, additive machines, and post-processing. Here we demonstrate the design and use of combinatorial samples produced on a commercial laser powder bed fusion system to study 60 distinct process conditions of nickel superalloy 625: five laser powers and four laser scan speeds in three different conditions. Combinatorial samples were characterized using optical and electron microscopy, x-ray diffraction, and indentation to estimate the porosity, grain size, crystallographic texture, secondary phase precipitation, and hardness. Indentation and porosity results were compared against a regular sample. The smaller-sized regions (3 mm × 4 mm) in the combinatorial sample have a lower hardness compared to a larger regular sample (20 mm × 20 mm) with similar porosity (< 0.03 %). Despite this difference, meaningful trends were identified with the combinatorial sample for grain size, crystallographic texture, and porosity versus laser power and scan speed as well as trends with hardness versus stress-relief condition.
Project description:Laser powder bed fusion (L-PBF) was attempted here to additively manufacture a new generation orthopedic β titanium alloy Ti-35Nb-7Zr-5Ta toward engineering patient-specific implants. Parts were fabricated using four different values of energy density (ED) input ranging from 46.6 to 54.8 J/mm3 through predefined laser beam parameters from prealloyed powders. All the conditions yielded parts of >98.5% of theoretical density. X-ray microcomputed tomography analyses of the fabricated parts revealed minimal imperfections with enhanced densification at a higher ED input. X-ray diffraction analysis indicated a marginally larger d-spacing and tensile residual stress at the highest ED input that is ascribed to the steeper temperature gradients. Cellular to columnar dendritic transformation was observed at the highest ED along with an increase in the size of the solidified features indicating the synergetic effects of the temperature gradient and solidification growth rate. Density measurements indicated ≈99.5% theoretical density achieved for an ED of 50.0 J/mm3. The maximum tensile strength of ≈660 MPa was obtained at an ED of 54.8 J/mm3 through the formation of the columnar dendritic substructure. High ductility ranging from 25 to 30% was observed in all the fabricated parts irrespective of ED. The assessment of cytocompatibility in vitro indicated good attachment and proliferation of osteoblasts on the fabricated samples that were similar to the cell response on commercially pure titanium, confirming the potential of the additively manufactured Ti-35Nb-7Zr-5Ta as a suitable material for biomedical applications. Taken together, these results demonstrate the feasibility of L-PBF of Ti-35Nb-7Zr-5Ta for potentially engineering patient-specific orthopedic implants.
Project description:We present a topological method for the detection and quantification of bone microstructure from non-linear microscopy images. Specifically, we analyse second harmonic generation (SHG) and two photon excited autofluorescence (TPaF) images of bone tissue which capture the distribution of matrix (fibrillar collagen) structure and autofluorescent molecules, respectively. Using persistent homology statistics with a signed Euclidean distance transform filtration on binary patches of images, we are able to quantify the number, size, distribution, and crowding of holes within and across samples imaged at the microscale. We apply our methodology to a previously characterized murine model of skeletal pathology whereby vascular endothelial growth factor expression was deleted in osteocalcin-expressing cells (OcnVEGFKO) presenting increased cortical porosity, compared to wild type (WT) littermate controls. We show significant differences in topological statistics between the OcnVEGFKO and WT groups and, when classifying the males, or females respectively, into OcnVEGFKO or WT groups, we obtain high prediction accuracies of 98.7% (74.2%) and 77.8% (65.8%) respectively for SHG (TPaF) images. The persistence statistics that we use are fully interpretable, can highlight regions of abnormality within an image and identify features at different spatial scales.