This paper addresses the effect of the post-process heat treatments on the microstructure and fatigue crack growth behaviour of the functionally graded (FG) laser powder bed fusion (L-PBF) Inconel 718 (IN718) superalloy. Sets of samples were additively manufactured (AM) altering the process parameters, namely the laser power, the laser scanning speed, layer thickness, hatch distance, and beam distribution function, resulting in distinctly different microstructures. Two categories of samples underwent heat treatment (HT) and hot isostatic pressing followed by HT (HIP+HT), while one category was kept in the as-processed (AP) condition to reveal the effects of the post-treatments. Additionally, to study the effect of microstructural anisotropy, samples were printed in horizontal (H) and vertical (V) building directions. To better understand the behaviour of the FG materials, non-graded (NG) L-PBF samples and wrought material were investigated as references. Significant variations in terms of porosity, grain size and elongation, crystallographic texture, and content of the strengthening precipitates or detrimental phases were found in different AM groups. The fatigue behaviour of the NG and FG materials was also studied by conducting three-point bending tests. Findings in terms of the role of different microstructures on the fatigue-crack initiation and fatigue crack growth rate are presented and discussed for all samples. The study demonstrated that heat treatments can enhance the damage tolerance of L-PBF IN718 to the level of wrought material. Interestingly, the effect of the roughness induced crack closure was found to be a function of build orientation, especially in the low stress ratio regime.

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Additive manufacturing of NiTi shape memory alloys has attracted attention in recent years, due to design flexibility and feasibility to achieve four-dimensional (4D) function response. To obtain customized 4D functional responses in NiTi structures, tailorable phase transformation temperatures and stress windows as well as one-way or two-way shape memory properties are required. To achieve this goal, various heat treatments, including direct aging, annealing and annealing followed by aging, were optimized for the Ti-rich NiTi (Ni49.6Ti (at. %)) fabricated by laser powder bed fusion (L-PBF). Microstructural evolution, phase transformation, precipitation and shape memory behaviour were systematically investigated by multiscale correlative microstructural, differential scanning calorimetry analysis and thermomechanical analysis. Based on optimized heat treatments, ∼25 K phase transformation temperature windows and ∼90 MPa stress windows were achieved for the one-way shape memory effect. Solutionized annealing was found to be the most effective way to improve one-way shape memory degradation resistance, due to the reduction of defects and solid solution strengthening. One of the main findings of this study is that the heterogonous microstructures between hard intergranular Ti₂NiO_x and soft NiTi matrix, induced by solutionized annealing with subsequent aging, result in strain partitioning and enclosing the internal stress state, which was found to promote a pronounced two-way shape memory effect response. The results of this work provide in-depth knowledge on tailoring and designing functional shape memory characteristics via heat treatments, which contributes to expanding L-PBF NiTi application fields, such as biomedical implants, aerospace components, and other advanced engineering applications.

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Electrochemical tests and surface analysis measurements were performed to study the corrosion behavior in a 0.9 wt.% NaCl solution at 37 °C of three NiTi shape memory alloys fabricated by laser-powder bed fusion (L-PBF). The passive film characteristics and corrosion resistance of L-PBF NiTi showed different features as a function of their preparation process settings. The passivation rate for L-PBF NiTi surfaces including defects, such as keyhole pores and cracks which showed high electrochemical activity accelerating the passivation reaction process, was higher in the early stages of immersion, but the corrosion resistance provided by such a rapidly formed passive film containing higher defect density is lower than that for an initially defect-free surface. The thickness of the passive film including a higher defect density does not necessarily relate to the corrosion resistance. The L-PBF NiTi prepared at a linear energy density of 0.2 J/m and volumetric energy density of 56 J/mm³ shows the least defects. Also, an outer Ti-rich and inner Ni-rich dense and corrosion protective passive film could be obtained for these L-PBF NiTi samples, which also results in a relatively low Ni ion release rate. A passive film model based on thickness, composition and defect density properties as a function of processing conditions is proposed to explain the difference in corrosion resistance of the various L-PBF NiTi.

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In energy absorption applications, architectured metallic materials generally suffer from unrecoverable deformation as a result of local yield damage or inelastic buckling. Nitinol (NiTi) offers recoverable deformation and energy dissipation due to its unique superelasticity, which can change the way we design and additively manufacture energy-absorbing architectured materials. The interplay between microstructure, mesoscopic deformation, and macroscopic thermomechanical response of NiTi architectured materials is still not studied in depth. In this work, NiTi architectured materials featuring anisotropic superelastic response, recoverable energy absorption and damping were successfully modeled and manufactured using laser powder bed fusion (L-PBF). Extensive numerical models demonstrated that NiTi architectured materials exhibit temperature-dependent superelasticity and effective transformation stress which can be controlled by the relative density and cell architecture. An effective transformation surface was developed based on the extended Hill's model, illustrating anisotropy is temperature-independent. Stable cyclic behavior with 2.8 % of reversible strain and damping behavior was successfully achieved in cyclic compressive tests without yielding damage or plastic buckling, which further illustrates that the progressive martensitic transformation is the main deformation and energy dissipation mechanism. A comparative study between designed herein body centered cubic (BCC) and octet structures showed that local microstructures significantly affect the deformation modes. The integrated computational and experimental study enables tailoring the superelasticity by combining structural design and microstructural control. Architectured materials designed in this study are potentially applicable as reusable impact absorbers in aerospace, automotive, maritime and vibration-proof structures.@en

Superelastic metallic materials possessing large recoverable strains are widely used in automotive, aerospace and energy conversion industries. Superelastic materials working at high temperatures and with a wide temperature range are increasingly required for demanding applications. Until recently, high-temperature superelasticity has only been achievable with multicomponent alloys fabricated by complex processes. In this study, a novel framework of multi-scale models enabling texture and microstructure design is proposed for high-performance NiTi fabrication via laser powder bed fusion. Based on the developed framework, a Ni-lean Ni(49.4 at.%)-Ti alloy is, for the first time, endowed with a 4% high-temperature compressive superelasticity. A 001 texture, unfavorable for plastic slip, is created to realize enhanced functionality. The unprecedented superelasticity can be maintained up to 453 K, which is comparable with but has a wider superelastic temperature range (∼110 K) than rare earth alloyed NiTi alloys, previously only realizable with grain refinement, and other complicated post-processing operations. At the same time, its shape memory stability is also improved due to existing textured 100 martensite and intergranular precipitation of Ti2NiOx. This discovery reframes the way that we design superior performance NiTi based alloys through directly tailoring crystallographic orientations during additive manufacturing.@en

In this paper, the effect of microstructural anisotropy on the fatigue crack growth behaviour of the functionally graded Inconel 718 fabricated through laser powder bed fusion (L-PBF) is investigated. Different manufacturing parameters, including low and high laser powers, were used to produce a variety of non-graded (NG) and functionally graded (G) specimens in two build directions, vertical and horizontal. In addition, a group of heat treated wrought samples was tested as a reference. It was observed that the different manufacturing parameters result in various grain size, crystallographic textures, precipitates and Laves phases, porosity, and un-melted particles. Three-point bending fatigue tests were conducted to measure the threshold stress intensity factor (ΔK_th) and fatigue crack growth rate (FCGR),da/dN. Only the lower laser power L-BPF Inconel material was found to have comparable to the wrought heat treated material fatigue crack growth behaviour. Furthermore, a new approach of automatically controlling ΔK as a function of the crack length was employed for graded specimens to investigate the crack growth rate as a function of local microstructure. The FCGR value of the vertical L-PBF samples, in which the crack direction was perpendicular to the build direction, remained constant. In contrast, the da/dN value of the horizontal samples with the crack direction parallel to the build direction increased constantly with the increase of the crack length. This behaviour is in good agreement with the hardness profile of the graded materials. Melt pool boundaries, graded interface boundaries, and grain orientations close to 〈001〉 were found to deflect the crack path. Additionally, it was found that L-PBF material is more affected (at a low stress ratio of R = 0.1) by the roughness-induced crack closure than the wrought counterparts. This study has successfully demonstrated the feasibility of using an additive manufacturing process to fabricate functionally graded materials featuring tailorable fatigue response of the local microstructures.

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The pursuit of enhancing NiTi superelasticity through laser powder bed fusion (L-PBF) and [001] texture creation poses a challenge due to increased susceptibility to hot cracking in the resulting microstructure with columnar grains. This limitation restricts NiTi's application and contributes to material waste. To overcome this, we introduce a pioneering approach: utilising spark plasma sintering (SPS) to heal directional cracks in [001] textured L-PBF NiTi shape memory alloy. Diffusion bonding and oxygen utilisation for Ti₂NiO_x formation was found to successfully heal the cracks. SPS enhances mechanical properties, superelasticity at higher temperatures, and two-way shape memory strain during thermomechanical cycling. This work provides an alternative solution for healing cracks in L-PBF parts, enabling the sustainable reuse of cracked materials. By implementing SPS, this approach effectively addresses hot cracking limitations, expanding the application potential of L-PBF NiTi parts while improving their functional and mechanical properties.

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Electrochemical tests and surface analysis were applied to study the corrosion behavior and passive film characteristics of three-dimensional-printed NiTi shape memory alloys fabricated by laser-powder bed fusion (L-PBF) in artificial saliva at 37 °C. The passivity of L-PBF NiTi shows to be influenced by the process parameters and resulting morphological and physicochemical surface properties. The results show that the defects at the surface of L-PBF NiTi can promote the passivation rate in the early stages of exposure but a slowly formed passive film shows the best corrosion protection. The thickness of the passive film is positively correlated with its corrosion protective performance. The L-PBF NiTi alloy prepared at a linear energy density of 0.2 J·m⁻¹ and volumetric energy density of 56 J·mm⁻³ shows the least defects and best corrosion protection. An outer Ti-rich and inner Ni-rich dense passive film could be also obtained showing higher corrosion resistance. Graphic Abstract: [Figure not available: see fulltext.]

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Nitinol (NiTi) shape memory alloys fabricated by Laser Powder Bed Fusion (L-PBF) Additive Manufacturing (AM) have attracted much attention in recent years, as compared with conventional manufacturing processes it allows to produce Nitinol parts with high design complexity. Avoidance of defects during L-PBF is crucial for the production of high quality Nitinol parts. In this study, analytical models predicting melt pool dimensions and defect formation criteria were synergistically used to develop processing maps demonstrating boundary conditions for the formation of such defects, as balling, keyhole-induced pores, and lack of fusion. Experimental validation has demonstrated that this method can provide an accurate estimation and guide manufacturability of defect-free Nitinol alloys. Moreover, the crack formation phenomena were experimentally analysed, which showed that a low linear energy density (E_l) should be chosen to avoid cracks in the optimized process windows. Based on model predictions and experimental calibrations, Nitinol samples with a relative density of more than 99% were successfully fabricated.

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The aim of this study was to determine the influence of selective laser melting (SLM) process parameters on the formation of cracks in nickel-based single crystal alloy. Several sets of laser scanning parameters, with varied laser power, scanning speed and hatch distance, thus resulting in different volumetric and linear energy densities, were investigated. The relationship between energy density, specimen densification, cracks formation and evolution of directional microstructure was shown. It was found that higher linear energy density results in fewer cracking and defects. Cracking in lower energy samples was attributed to the formation of thermal shrinkage pores in the interdendritic spaces and precipitation of Ta, Mo and Nb carbides along the dendrites boundaries.@en

The aim of this study was to determine the influence of heat treatment on the microstructure of single-crystal nickel-based alloy manufactured by selective laser melting with a high-temperature substrate preheating. The change of gamma/gamma prime -phases ratio was established as a result of various heat treatment modes.

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The paper investigates the effect of hot isostatic pressing of single-crystal nickel-based alloy manufactured by selective laser melting (SLM) with a high-temperature substrate preheating. A study of the structure and phase composition of the material before and after treatment has been carried out. It was found that as a result of such treatment, the ratio and proportion of the strengthening phases change; however, due to slow cooling after treatment, the optimal ratio and shape of the inclusions are not fixed. In addition, the hardening particles are precipitated.@en

Selective laser melting (SLM) process has been lately extensively applied in manufacturing of Nickel-based super alloys, which compared to conventional manufacturing routes offers increased design flexibility and simplification of the manufacturing process. However, in order to make SLM process even more beneficial, its process time has to be reduced. One of the ways to tackle this problem is by tailoring process parameters through application of high laser power and base plate pre-heating. In this paper, a comparative study of optimum SLM fabrication conditions of Inconel 718 superalloy under high laser power and with and without plate pre-heating was conducted. Furthermore, the effect of layer thickness on melt pool characteristics, porosity and hardness were investigated to determine how laser power and pre-heating affect microstructure development. @en

This work investigates Selective Laser Melting (SLM) process as a method of in-situ synthesis of Ti-5Al and Ti-6Al-4V alloys using elemental powder mixture. Elemental spherical powders were used to prepare a powder mixture and the samples were produced by SLM process using different volume energy densities. The effects of volume energy density on the samples’ relative density, chemical composition, microstructure and microhardness before and after heat treatment have been studied. It was shown that volume energy density significantly effects the density and microstructure of Ti-5Al and Ti-6Al-4V alloys, as well as, the microhardness of obtained Ti-6Al-4V.@en

The paper presents the study results of the selective laser melting process of the Ti-6Al-4V alloy and nanosized powder TiC composition. The results of the particles morphology study of resulting powder composition after blending are presented. The microstructure and mechanical characteristics of the obtained composite material were studied. Study of microstructures using optical and electron microscopes were conducted.

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Laser powder bed fusion (L-PBF), categorized as additive manufacturing technique, has a capability to fabricate NiTi (Nitinol) shape memory alloys with tailorable functional properties and complex geometries. An important processing parameter, hatch distance (h), is often related to macroscale structural defects; however, its role on controlling the microstructure and functional properties is usually underestimated in L-PBF of NiTi. In this work, equiatomic NiTi (50.0 at% Ni) parts were fabricated with various hatch distances to tailor the microstructure and their shape memory characteristics. Contrary to what is observed in Ni-rich NiTi alloys, in this work, we demonstrate that phase transformation temperatures of L-PBF equiatomic NiTi do not decrease proportionally with hatch distance but rather relate to a critical hatch distance value. This critical value (120 μm) is derived from the synergistic effect of thermal stress and in situ reheating. Below this value, epitaxial grain growth and in situ recrystallization are enhanced, while above, irregular grains are formed and dislocations induced by thermal stresses decrease. However, the critical value found herein is characterized by high dislocation density and fine grain size, resulting in a superior thermal cyclic stability. The proposed finite element model is proven to be an effective tool to understand and predict the effect of hatch distance on grain morphology and dislocation density evolutions in L-PBF NiTi SMAs. In the present study, we provide a comprehensive understanding for in situ controlling L-PBF NiTi microstructure and functional characteristics, which contributes to designing 4-dimensional shape memory alloys.

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