Microstructure of TiAl Capsules Processed by Electron Beam Powder Bed Fusion Followed by Post-Hot Isostatic Pressing.

The microstructures of intermetallic γ-titanium aluminide (TiAl) alloys are subjected to a certain degree of Al evaporation when processed by electron beam powder bed fusion (EB-PBF). The magnitude of the Al-loss is mainly correlated with the process parameters, and highly energetic parameters produce significant Al evaporation. The Al-loss leads to different microstructures, including the formation of inhomogeneous banded structures, thus negatively affecting its mechanical performance. For this reason, the current work deals with creating EB-PBFed TiAl capsules with the inner part produced using only the pre-heating step and melting parameters with low energetic parameters applying high beam speed from 5000 to 3000 mm/s. This approach is investigated to reduce the Al-loss and microstructure inhomogeneity after hot isostatic pressing (HIP). The results showed that the HIP treatment effectively densified the capsules obtaining a relative density of around 100%. After HIP, the capsules produced with the inner part melted at 3000 mm/s presented a lower area shrinkage (around 6.6%) compared to the capsules produced using only the pre-heating step in the core part (around 20.7%). The different magnitudes of shrinkage derived from different levels of residual porosity consolidated during the HIP process. The HIPed capsules exhibited the presence of previous particle boundaries (PPBs), covered by α2 phases. Notably, applying low energetic parameters to melt the core partially eliminates the particles' surface, thus reducing the PPBs formation. In this case, the capsules melted with low energetic parameters (3000 mm/s) exhibited α2 concentration of 3.5% and an average size of 13 µm compared to the capsules produced with the pre-heating step in the inner part with an α2 around 5.7% and an average size around 23 µm. Moreover, the Al-loss of the capsules was drastically limited, as determined by X-ray fluorescence (XRF) analysis. More in detail, the capsules produced with the pre-heating step reported an atomic percentage of Al of 48.75, while using low energetic melting parameters led to 48.36. This result was interesting, considering that the massive samples produced with standard parameters (so more energetic ones) revealed atomic Al percentage from 48.04 to 47.70. Finally, the recycled small particles showed a higher fraction of α2 phases with respect to the coarse particles, as determined by X-ray diffraction (XRD).

Low-Power Laser Powder Bed Fusion Processing of Scalmalloy®.

Among recently developed high-strength and lightweight alloys, the high-performance Scalmalloy® certainly stands out for laser powder bed fusion (LPBF) production. The primary goal of this study was to optimize the Scalmalloy® LPBF process parameters by setting power values suitable for the use of lab-scale machines. Despite that these LPBF machines are commonly characterized by considerably lower maximum power values (around 100 W) compared to industrial-scale machines (up to 480 W), they are widely used when quick setup and short processing time are needed and a limited amount of powder is available. In order to obtain the optimal process parameters, the influence of volumetric energy density (VED) on the sample porosity, microstructure and mechanical properties was accurately studied. The obtained results reveal the stability of the microstructural and mechanical behaviour of the alloy for VEDs higher than 175 Jmm-3. In this way, an energy-and-time-saving choice at low VEDs can be taken for the LPBF production of Scalmalloy®. After identifying the low-power optimized process parameters, the effects of the heat treatment on the microstructural and mechanical properties were investigated. The results prove that low-VED heat-treated samples produced with an LPBF lab-scale machine can achieve outstanding mechanical performance compared with the results of energy-intensive industrial production.

Effect of Aging and Cooling Path on the Super ß-Transus Heat-Treated Ti-6Al-4V Alloy Produced via Electron Beam Melting (EBM).

This work focuses on the effect of different heat treatments on the Ti-6Al-4V alloy processed by means of electron beam melting (EBM). Super ß-transus annealing was conducted at 1050 °C for 1 h on Ti-6Al-4V samples, considering two different cooling paths (furnace cooling and water quenching). This heat treatment induces microstructural recrystallization, thus reducing the anisotropy generated by the EBM process (columnar prior-ß grains). Subsequently, the annealed furnace-cooled and water-quenched samples were aged at 540 °C for 4 h. The results showed the influence of the aging treatment on the microstructure and the mechanical properties of the annealed EBM-produced Ti-6Al-4V. A comparison with the traditional processed heat-treated material was also conducted. In the furnace-cooled specimens consisting of lamellar α+ß, the aging treatment improved ductility and strength by inducing microstructural thickening of the α laths and reducing the ß fraction. The effect of the aging treatment was also more marked in the water-quenched samples, characterized by high tensile strengths but limited ductility due to the presence of martensite. In fact, the aging treatment was effective in the recovery of the ductility loss, maintaining high tensile strength properties due to the variation in the relative number of α/α' interfaces resulting from α' decomposition. This study, therefore, offers an in-depth investigation of the potential beneficial effects of the aging treatment on the microstructure and mechanical properties of the EBM-processed super ß-transus heat-treated Ti-6Al-4V alloy under different cooling conditions.

Stress Corrosion Cracking of Additively Manufactured Alloy 625.

Laser bed powder fusion (LPBF) is an additive manufacturing technology for the fabrication of semi-finished components directly from computer-aided design modelling, through melting and consolidation, layer upon layer, of a metallic powder, with a laser source. This manufacturing technique is particularly indicated for poor machinable alloys, such as Alloy 625. However, the unique microstructure generated could modify the resistance of the alloy to environment assisted cracking. The aim of this work was to analyze the stress corrosion cracking (SCC) and hydrogen embrittlement resistance behavior of Alloy 625 obtained by LPBF, both in as-built condition and after a standard heat treatment (grade 1). U-bend testing performed in boiling magnesium chloride at 155 and 170 °C confirmed the immunity of the alloy to SCC. However, slow strain rate tests in simulated ocean water on cathodically polarized specimens highlighted the possibility of the occurrence of hydrogen embrittlement in a specific range of strain rate and cathodic polarization. The very fine grain size and dislocation density of the thermally untreated specimens appeared to increase the hydrogen diffusion and embrittlement effect on pre-charged specimens that were deformed at the high strain rate. Conversely, heat treatment appeared to mitigate hydrogen embrittlement at high strain rates, however at the slow strain rate all the specimens showed a similar behavior.

Electron Backscattered Diffraction to Estimate Residual Stress Levels of a Superalloy Produced by Laser Powder Bed Fusion and Subsequent Heat Treatments.

Metal Additive Manufacturing and Laser Powder Bed Fusion (LPBF), in particular, have come forth in recent years as an outstanding innovative manufacturing approach. The LPBF process is notably characterized by very high solidification and cooling rates, as well as repeated abrupt heating and cooling cycles, which generate the build-up of anisotropic microstructure and residual stresses. Post-processing stress-relieving heat treatments at elevated temperatures are often required in order to release some of these stresses. The effects of 1 h-hold heat treatments at different specific temperatures (solutionizing, annealing, stress-relieve and low-temperature stress-relieve) on residual stress levels together with microstructure characterization were therefore investigated for the popular Alloy 625 produced by LPBF. The build-up of residual stress is accommodated by the formation of dislocations that produce local crystallographic misorientation within grains. Electron backscattered diffraction (EBSD) was used to investigate local misorientation by means of orientation imaging, thereby assessing misorientation or strain levels, in turn representing residual stress levels within the material. The heavily constrained as-built material was found to experience full recrystallization of equiaxed grains after solutionizing at 1150 °C, accompanied by significant drop of residual stress levels due to this grains reconfiguration. Heat treatments at lower temperatures however, even as high as the annealing temperature of 980 °C, were found to be insufficient to promote recrystallization though effective to some extent to release residual stress through apparently dislocations recovery. Average misorientation data obtained by EBSD were found valuable to evaluate qualitatively residual stress levels. The effects of the different heat treatments are discussed and suggest that the peculiar microstructure of alloys produced by LPBF can possibly be transformed to suit specific applications.

Correction: Bassini,~E.; et al. Study of the Effects of Aging Treatment on Astroloy Processed via Hot Isostatic Pressing. Materials 2019, 12, 1517.

The authors wish to make the following correction to the paper [...].

Microstructural Evolution of Post-Processed Hastelloy X Alloy Fabricated by Laser Powder Bed Fusion.

Hastelloy X (HX) is a Ni-based superalloy which is employed to produce gas turbine and gas-cooled reactor sectors due to its outstanding oxidation resistance and high tensile strength at high temperatures. This alloy can be processed by laser powder bed fusion (LPBF) fabricating complex geometries in a single step. However, post-processing thermal treatments must be applied to generate a suitable microstructure for high-temperature applications. The investigation reports the microstructure evolution of LPBF HX samples under specific post-processing treatments. A hot isostatic pressing (HIP) treatment can close the internal cracks and reduce the residual porosity (less than 0.1%). Moreover, the HIP-triggered recrystallization generated equiaxed grains, while the slow cooling rate generated a film of intergranular carbides (Mo-rich M6C and Cr-rich M23C6) and intragranular carbides (Mo-rich M6C carbides). Therefore, a solution annealing was performed to dissolve the film of carbides which may reduce the ductility. The post solution annealed material consisted of equiaxed grains with ASTM grain size number mainly 4.5-5.5 and inter/intragranular Mo-rich M6C carbides. The microstructure is highly comparable with solution annealed wrought HX alloy. Finally, after simulating short thermal exposure at 745 °C for 6 h, a significant formation of Cr-rich M23C6 carbides was observed strengthening the LPBF HX alloy.

New Aluminum Alloys Specifically Designed for Laser Powder Bed Fusion: A Review.

Aluminum alloys are key materials in additive manufacturing (AM) technologies thanks to their low density that, coupled with the possibility to create complex geometries of these innovative processes, can be exploited for several applications in aerospace and automotive fields. The AM process of these alloys had to face many challenges because, due to their low laser absorption, high thermal conductivity and reduced powder flowability, they are characterized by poor processability. Nowadays mainly Al-Si alloys are processed, however, in recent years many efforts have been carried out in developing new compositions specifically designed for laser based powder bed AM processes. This paper reviews the state of the art of the aluminum alloys used in the laser powder bed fusion process, together with the microstructural and mechanical characterizations.

Study of the Effects of Aging Treatment on Astroloy Processed via Hot Isostatic Pressing.

The effect of aging treatment on Astroloy fabricated via hot isostatic pressing and subjected to super-, and sub- solvus solutioning has been investigated. The evolution of hardness and microstructural features were followed after each step of the treatment. Since this alloy is commonly subjected to a double aging treatment at two different temperatures, particular attention was given to the effectiveness of the first aging treatment compared to the second one. Coarsening and modification of the γ' reinforcing system together with carbides formation were made the object of research. The cooling rate used after solutioning treatment was also kept into account. Finally, a model to describe secondary and ternary gamma prime coarsening upon aging treatments is presented.

Microstructure and Selective Corrosion of Alloy 625 Obtained by Means of Laser Powder Bed Fusion.

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.

Study of the Microstructure and Cracking Mechanisms of Hastelloy X Produced by Laser Powder Bed Fusion.

Hastelloy X (HX) is a Ni-based superalloy which suffers from high crack susceptibility during the laser powder bed fusion (LPBF) process. In this work, the microstructure of as-built HX samples was rigorously investigated to understand the main mechanisms leading to crack formation. The microstructural features of as-built HX samples consisted of very fine dendrite architectures with dimensions typically less than 1 µm, coupled with the formation of sub-micrometric carbides, the largest ones were mainly distributed along the interdendritic regions and grain boundaries. From the microstructural analyses, it appeared that the formation of intergranular carbides provided weaker zones, which combined with high thermal residual stresses resulted in hot cracks formation along the grain boundaries. The carbides were extracted from the austenitic matrix and characterized by combining different techniques, showing the formation of various types of Mo-rich carbides, classified as M6C, M12C and MnCm type. The first two types of carbides are typically found in HX alloy, whereas the last one is a metastable carbide probably generated by the very high cooling rates of the process.

Characterization of an Additive Manufactured TiAl Alloy-Steel Joint Produced by Electron Beam Welding.

In this work, the characterization of the assembly of a steel shaft into a γ-TiAl part for turbocharger application, obtained using Electron Beam Welding (EBW) technology with a Ni-based filler, was carried out. The Ti-48Al-2Nb-0.7Cr-0.3Si (at %) alloy part was produced by Electron Beam Melting (EBM). This additive manufacturing technology allows the production of a lightweight part with complex shapes. The replacement of Nickel-based superalloys with TiAl alloys in turbocharger automotive applications will lead to an improvement of the engine performance and a substantial reduction in fuel consumption and emission. The welding process allows a promising joint to be obtained, not affecting the TiAl microstructure. Nevertheless, it causes the formation of diffusive layers between the Ni-based filler and both steel and TiAl, with the latter side being characterized by a very complex microstructure, which was fully characterized in this paper by means of Scanning Electron Microscopy, Energy Dispersive X-ray Spectroscopy, and nanoindentation. The diffusive interface has a thickness of about 6 µm, and it is composed of several layers. Specifically, from the TiAl alloy side, we find a layer of Ti3Al followed by Al3NiTi2 and AlNi2Ti. Subsequently Ni becomes more predominant, with a first layer characterized by abundant carbide/boride precipitation, and a second layer characterized by Si-enrichment. Then, the chemical composition of the Ni-based filler is gradually reached.

Additive manufacturing of titanium alloys in the biomedical field: processes, properties and applications.

The mechanical properties and biocompatibility of titanium alloy medical devices and implants produced by additive manufacturing (AM) technologies - in particular, selective laser melting (SLM), electron beam melting (EBM) and laser metal deposition (LMD) - have been investigated by several researchers demonstrating how these innovative processes are able to fulfil medical requirements for clinical applications. This work reviews the advantages given by these technologies, which include the possibility to create porous complex structures to improve osseointegration and mechanical properties (best match with the modulus of elasticity of local bone), to lower processing costs, to produce custom-made implants according to the data for the patient acquired via computed tomography and to reduce waste.

Effect of ZrB2 addition on the oxidation behavior of Si-SiC-ZrB2 composites exposed at 1500°C in air.

BACKGROUND: Silicon carbide ceramics obtained by reactive infiltration of silicon (SRI) have many industrial applications especially involving severe and high temperature conditions. In this study, the oxidation behavior in air of Si-SiC-ZrB2 systems at a high temperature (1500°C) for dwelling times of up to 48 hours was examined. METHODS: The oxidation process was analyzed on the basis of elemental maps and X-ray diffraction patterns taken, respectively, on the core and on the surface of the specimens, together with weight gains and the average thicknesses of the resulting scale. Further, flexural strength at room temperature was examined as a function of different oxidation times. RESULTS: The main chemical reactions and phase transformations involved in the oxidation process are reported. Several oxides were detected on the surface: zirconia, silica, zircon and 3-zirconium monoxide. All of the samples showed a parabolic oxidation kinetics, suggesting that the controlling mechanism was the diffusion; however, even after 48 hours, the oxidation process was not finished - indeed, all of the samples continued to gain weight. CONCLUSIONS: The oxidation of Si-SiC-ZrB2 material produced via SRI was slower compared with previously investigated ZrB2-SiC composites processed with a different techniques and tested in similar conditions. The oxidation mechanism was found to be consistent with the convection cells model.

Production of Single Tracks of Ti-6Al-4V by Directed Energy Deposition to Determine the Layer Thickness for Multilayer Deposition.

Directed Energy Deposition (DED), which is an additive manufacturing technique, involves the creation of a molten pool with a laser beam where metal powder is injected as particles. In general, this technique is employed to either fabricate or repair different components. In this technique, the final characteristics are affected by many factors. Indeed, one of the main tasks in building components by DED is the optimization of process parameters (such as laser power, laser speed, focus, etc.) which is usually carried out through an extensive experimental investigation. However, this sort of experiment is extremely lengthy and costly. Thus, in order to accelerate the optimization process, an investigation was conducted to develop a method based on the melt pool characterizations. In fact, in these experiments, single tracks of Ti-6Al-4V were deposited by a DED process with multiple combinations of laser power and laser speed. Surface morphology and dimensions of single tracks were analyzed, and geometrical characteristics of melt pools were evaluated after polishing and etching the cross-sections. Helpful information regarding the selection of optimal process parameters can be achieved by examining the melt pool features. These experiments are being extended to characterize the larger blocks with multiple layers. Indeed, this manuscript describes how it would be possible to quickly determine the layer thickness for the massive deposition, and avoid over or under-deposition according to the calculated energy density of the optimum parameters. Apart from the over or under-deposition, time and materials saving are the other great advantages of this approach in which the deposition of multilayer components can be started without any parameter optimization in terms of layer thickness.

Thermal Shock and Oxidation Behavior of HiPIMS TiAlN Coatings Grown on Ti-48Al-2Cr-2Nb Intermetallic Alloy.

A High Power Impulse Magnetron Sputtering (HiPIMS) method for depositing TiAlN environmental barrier coatings on the surface of Ti-48Al-2Cr-2Nb alloy was developed in view of their exploitation in turbine engines. Three differently engineered TiAlN films were processed and their performance compared. Bare intermetallic alloy coupons and coated specimens were submitted to thermal cycling under oxidizing atmosphere up to 850 °C or 950 °C, at high heating and cooling rates. For this purpose, a burner rig able to simulate the operating conditions of the different stages of turbine engines was used. Microstructures of the samples were compared before and after each test using several techniques (microscopy, XRD, and XPS). Coating-intermetallic substrate adhesion and tribological properties were investigated too. All the TiAlN films provided a remarkable increase in oxidation resistance. Good adhesion properties were observed even after repeated thermal shocks. HiPIMS pretreatments of the substrate surfaces performed before the coating deposition significantly affected the oxidation rate, the oxide layer composition and the coating/substrate adhesion.