Additively manufactured Nitinol (NiTi) architectured materials, designed with unit cell architectures, hold promise for customisable applications. However, the common assumption of homogeneity in modeling and additive manufacturing of these architectured materials needs further investigation because geometric-dependent melt pool behaviour results in inhomogeneous microstructure and thermomechanical properties. This study shows that property inhomogeneity at the mesoscale is one reason for pseudo-linear response and partial superelasticity of the fabricated NiTi body-centered cubic (BCC) architectured materials. We modeled using a phenomenological constitutive relation and additively manufactured NiTi architectured materials with varying relative densities. These fabricated samples showed distinct microstructural textures and compositions that affected their local recoverability. The edge effects and laser turn regions were identified as the causes underlying the observed microstructural inhomogeneity. The dimensionless Fourier number is used to describe the transition of printing modes. This study provides valuable information on rigorous experimental/computational consistency in future work.

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High strength steels are widely used for structural applications, where a combination of excellent strength and ductile-to-brittle transition (DBT) properties are required. However, such a combination of high strength and toughness can be deteriorated in the heat affected zone (HAZ) after welding. This work aims to develop a relationship between microstructure and cleavage fracture in the most brittle areas of welded S690 high strength structures: coarse-grained and intercritically reheated coarse-grained HAZ (CGHAZ and ICCGHAZ). Gleeble thermal simulations were performed to generate three microstructures: CGHAZ and ICCGHAZ at 750 and 800 °C intercritical peak temperatures. Their microstructures were characterised, and the tensile and fracture properties were investigated at − 40 °C, where cleavage is dominant. Results show that despite the larger area fraction of martensite-austenite (M-A) constituents in ICCGHAZ 750 °C, the CGHAZ is the zone with the lowest fracture toughness. Although M-A constituents are responsible for triggering fracture, their small size (less than 1 μm) results in local stress that is insufficient for fracture. Crack propagation is found to be the crucial fracture step. Consequently, the harder auto-tempered matrix of CGHAZ leads to the lowest fracture toughness. The main crack propagates transgranularly, along {100} and {110} planes, and neither the necklace structure at prior austenite grain boundaries of ICCGHAZs nor M-A constituents are observed as preferential sites for crack growth. The fracture profile shows that prior austenite grain boundaries and other high-angle grain boundaries (e.g., packet and block) with different neighbouring Bain axes can effectively divert the cleavage crack. Moreover, M − A constituents with internal sub-structures, which have high kernel average misorientation and high-angle boundaries, are observed to deflect and arrest the secondary cracks. As a result, multiple pop-ins in load-displacement curves during bending tests are observed for the investigated HAZs.

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This study investigated the in-situ gaseous (under 150 bar) hydrogen embrittlement behaviour of additively manufactured (AM) Inconel 718 produced from sustainable feedstock. Here, sustainable feedstock refers to the Inconel 718 powder produced by vacuum induction melting inert gas atomisation of failed printed parts or waste from CNC machining. All Inconel 718 samples, namely AM-as-processed, AM-heat-treated and conventional samples showed severe hydrogen embrittlement. Additionally, it was found that despite its higher yield strength (1462 ± 8 MPa) and the presence of δ phase, heat-treated AM Inconel 718 demonstrates 64% lower degree of hydrogen embrittlement compared to the wrought counterpart (Y.S. 1069 ± 4 MPa). This was linked to the anisotropic microstructure induced by the AM process, which was found to cause directional embrittlement unlike the wrought samples showing isotropic embrittlement. In conclusion, this study shows that AM Inconel 718 produced from recycled feedstock shows better hydrogen embrittlement resistance compared to the wrought sample. Furthermore, the unique anisotropic properties, seen in this study for Inconel 718 manufactured by laser powder bed fusion, could be considered further in component design to help minimise the degree of hydrogen embrittlement.@en

Sub-size specimen testing offers a potentially elegant solution to accompany fatigue life assessments in determining vital fatigue parameters such as effective fatigue crack growth propagation thresholds (ΔK_th,eff). Additively manufactured parts stand to benefit from this in potential build-by-build fatigue validation without foregoing process-inherent material saving and low lead times. In this study, sub-size Laser Powder Bed Fusion (LPBF) produced Ti-6Al-4 V SENB specimens built in two orientations with stress relieved and annealed material states are considered. Scanning electron microscopy with electron backscatter diffraction is used to consider both meso- and microstructural features, complimented by digital image correlation (DIC) for determining local stress intensity and triaxiality around the crack tip. Results show inconsistent near-threshold fatigue behaviour linked to the microstructure of annealed material, where the fatigue threshold in sub-size specimens is reduced. Furthermore, reducing specimen size influences both in- and out-of-plane crack tip constraint, with higher constraint experienced by the sub-size specimens. Overall, this study presents and discusses the domain and suitability in using sub-size specimen FCGR threshold testing for LPBF produced Ti-6Al-4 V builds considering their unique meso- and microstructural features.

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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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In this work, the hydrogen fatigue of pipeline steel X60, its girth welds and weld defects were investigated through in situ fatigue testing. A novel in situ gaseous hydrogen charging fatigue set-up was developed, which involves a sample geometry that mimics a small-scale pipeline with high internal hydrogen gas pressure. The effect of hydrogen was investigated by measuring the crack initiation and growth, using a direct current potential drop (DCPD) set-up, which probes the outer surface of the specimen. The base and weld metal specimens both experienced a reduction in fatigue life in the presence of hydrogen. For the base metal, the reduction in fatigue life manifested solely in the crack growth phase; hydrogen accelerated the crack growth by a factor of 4. The crack growth rate for the weld metal accelerated by a factor of 8. However, in contrast to the base metal, the weld metal also experienced a reduction of 57% in resistance to crack initiation. Macropores (>500 µm in size) on the notch surface reduced the fatigue life by a factor of 11. Varying the pressure from 70 barg to 150 barg of hydrogen caused no difference in the hydrogen fatigue behavior of the weld metal. The fracture path of the base and weld metal transitioned from transgranular and ductile in nature to a mixed-mode transgranular and intergranular quasi-cleavage fracture. Hydrogen accelerated the crack growth by decreasing the roughness- and plasticity-induced crack closure. The worst case scenario for pipelines was found in the case of weld defects. This work therefore highlights the necessity to re-evaluate pipelines for existing defects before they can be reused for hydrogen transport.@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.

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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.

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The reversible behaviour of metals at low applied stresses is more complex than the generally assumed linear behaviour. This is primarily because of the reversible nature of dislocation motion leading to a strain contribution known as anelasticity. This work aims to investigate (a) quantification of dislocation structures in industrial grade stainless steels, (b) unloading behaviour, and (c) the fundamentals of reversible and mechanical behaviour occurring below the yield stress. Mechanical testing of martensitic stainless steel (Stavax ESR) was performed in two different modes: incremental plastic deformation and cyclic loading-unloading below the yield stress with a focus on the measurement of small strains and corresponding stresses, occurring in the pre-yield regime. The non-linear reversible behaviour was quantitatively analysed, as opposed to the common approximation of an empirical determination of apparent Young's modulus. The recently proposed pre-yield model has been refined and, for the first time, successfully applied to a complex microstructure such as stainless steel. The quantification of dislocation structure parameters is shown to be an efficient alternative to the conventional experimental methods of quantifying dislocation structure. Further, a unique representation and quantification of the unloading and hysteresis behaviour provides more insight into the material behaviour. Lastly, the little studied microplasticity occurring below the yield stress upon cyclic loading-unloading was determined. Importantly, the physical basis of the model will allow quantification of plastic deformations in the pre-yield region, large enough to be significant in industrial processes.

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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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With fossil fuels being phased out and growing global interest in a hydrogen economy, there is demand for re-purposing existing pipelines for transportation of hydrogen gas. However, hydrogen embrittlement (HE) can limit pipeline steel’s performance. In this study, the effect of hydrogen on the mechanical properties of an X60 base metal (polygonal ferrite/pearlite) and its girth weld (acicular ferrite/pearlite) was measured with a novel slow strain rate tensile (SSRT) test in which hollow pipe-like specimens were internally pressurised with nitrogen and hydrogen gas from 0 to 100 bars. Results showed that exposure to H₂ gas at 100 bars reduced the ductility of the base metal by up to 40% and the weld metal by 14%. Reduction in cross-sectional area (%RA) reduced by up to 28% in the base metal and 11% in the weld metal. Fracture surface analysis showed micro-void coalescence as well as quasi-cleavage fracture characteristic of HE. Susceptibility to HE was also observed in the form of secondary longitudinal and internal transverse cracks.

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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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This work discusses the design and demonstration of an in-situ test setup for testing pipeline steels in a high pressure gaseous hydrogen (H2) environment. A miniature hollow pipe-like tensile specimen was designed that acts as the gas containment volume during the test. Specific areas of the specimen can be forced to fracture by selective notching, as performed on the weldment. The volume of H2 used was minimised so the test can be performed safely without the need of specialised equipment. The setup is shown to be capable of characterising Hydrogen Embrittlement (HE) in steels through testing an X60 pipeline steel and its weldment. The percentage elongation (%El) of the base metal was found to be reduced by 40% when tested in 100 barg H2. Reduction of cross-sectional area (%RA) was found to decrease by 28% and 11% in the base metal and weld metal, respectively, when tested in 100 barg H2. Benchmark test were performed at 100 barg N2 pressure. SEM fractography further indicated a shift from normal ductile fracture mechanisms to a brittle transgranular (TG) quasi-cleavage (QC) type fracture that is characteristic of HE.@en

In previous work on the thermo-mechanical fatigue (TMF) of compacted graphite iron (CGI), lifetimes measured under total constraint were confirmed analytically by numerical integration of Paris’ crack-growth law. In current work, the results for CGI are further validated for spheroidal cast iron (SGI), while TMF tests at different constraint levels were additionally performed. The Paris crack-growth law is found to require a different CParis parameter value per distinct constraint level, indicating that Paris’ law does not capture all physical backgrounds of TMF crack growth, such as the effect of constraint level. An adapted version of Paris’ law is developed, designated as the local strain model. The new model considers cyclic plastic strains at the crack tip to control crack growth and is found to predict TMF lifetimes of SGI very well for all constraint levels with a single set of parameters. This includes not only full constraint but also over and partial constraint conditions, as encountered in diesel engine service conditions. The local strain model considers the crack tip to experience a distinct sharpening and blunting stage during each TMF cycle, with separate contributions to crack-tip plasticity, originating from cyclic bulk stresses in the sharpening stage and cyclic plastic bulk strains in the blunting stage. @en

The fracture toughness of high strength steels is commonly determined by standard methods using Compact tension (CT) or Single edge notched bend (SENB) specimens. In the past the Circumferentially Notched Tension (CNT) geometry has been reported as a potential candidate for determining the fracture toughness of highly constrained cracks, theoretically approaching plane strain conditions, even for small specimen dimensions. The goal of this study is to develop a more fundamental understanding of the CNT methodology and apply it to high strength S690QT steel. An alternative prefatiguing method was developed and a straightforward relation was established between the Crack Mouth Opening Displacement (CMOD) and the Crack Tip Opening Displacement (CTOD). With the new experimental aspects, it proved feasible to determine upper-shelf CTOD values for S690QT steel, using small CNT specimens (D = 12 mm), tested at room temperature with a relative high loading rate. Furthermore, CNT low temperature values were found comparable to those of conventional SENB tests. Hence, the research demonstrates that CNT geometry allows for small scale high loading rate specimen testing, resulting in simple, rapid and cost effective fracture toughness determination.@en

Inconel 718 is a nickel-based superalloy commonly used in aircraft engine and nuclear applications, where components experience severe mechanical stresses. Due to the typical high temperature applications, Thermo-Mechanical Fatigue (TMF) and creep tests are common benchmarks for such applications. Additive manufacturing offers a unique way of manufacturing Inconel 718 with high degree of design freedom. However, limited knowledge exists regarding the resulting high temperature properties. The objective of this work is to evaluate creep and TMF behaviour of Inconel 718, produced by selective laser melting (SLM). A novel microstructural design, allowing for grain size control was employed in this study. The obtained functionally graded Inconel 718, exhibiting core with coarse and outside shell with fine grained microstructure, allowed for the best trade-off between creep and fatigue performance. The post heat-treatment regimens and resulting microstructures are also evaluated and its influence on creep and TMF is discussed.

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Orientation contrast microscopy (i.e., electron backscattered diffraction, EBSD) was employed to monitor the plastic strain in loaded tensile samples of aluminium alloy Al6061 in T4 condition. The kernel average misorientation (KAM) is known to be an appropriate parameter in orientation contrast microscopy which has the potential to characterise the plastic strain by monitoring the local misorientations. This technique was applied here to gauge the extent of the plastic zone around a fatigue crack. To establish the magnitude of strain (which can be identified by the KAM parameter), a series of tensile samples were strained in the range of 1% to 25%. KAM maps were compared, and the average misorientations were related to the tensile strain values. The KAM distribution functions for all the strained samples were derived from a large scanned area. In addition, Vickers microhardness tests were conducted for these series of samples. This allowed the comparison of the mesoscopic plastic strain measured by Vickers microhardness with the micro plastic strain locally obtained by KAM. Noise was observed in the average KAM values up to a plastic strain of 1.5%. For the plastic strain exceeding 1.5%, noise no longer dominates the KAM map, and a positive—though not linear—correspondence between plastic strain and KAM was observed. The observed plastic zone at the tip of the fatigue crack by micro-Vickers hardness measurements was about an order of magnitude higher than the plastic zone observed on the KAM maps. In view of the calibration of KAM values on the tensile samples, it could be concluded that in the larger area of the plastic zone, the strain did not exceed the critical value of 1.5%@en

The possibility of using a mix of recycled polypropylene (PP) with new glass fibre reinforced polypropylene as a materials source for 3D printed engineering components is investigated. The strength and elongation to fracture are determined for various grades of material and in relation to the print direction. The measured values are compared with literature values for these materials in an as new condition. It is shown that the use of recycled PP degrades the material properties. PP recycled from house hold waste has significantly worse properties than PP recycled from industrial waste.@en