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Green Open Access added to TU Delft Institutional Repository 'You share, we take care!' - Taverne project https://www.openaccess.nl/en/you-share-we-take-care Otherwise as indicated in the copyright section: the publisher is the copyright holder of this work and the author uses the Dutch legislation to make this work public., Team Vera Popovich

Shape memory alloys (SMAs), such as nickel-titanium (NiTi) alloys or Nitinol, possess remarkable properties, including superelasticity and shape memory effects, which are attributed to the reversible martensitic transformation. However, traditional manufacturing of NiTi SMAs is challenging due to its high ductility and reactivity, which limits NiTi applications to simple geometries. In this context, laser powder bed fusion (L-PBF), an additive manufacturing technique, emerges as a promising solution capable of overcoming these limitations and introducing the concept of four-dimensional (4D) printing. This approach enables the creation of morphing shapes that can be activated by external stimuli, such as heat or stress, particularly beneficial for SMAs., Team Vera Popovich

Boron containing MoSi2 is a promising material for applications at high temperature, but the oxidation mechanism is still unclear. In this work, the high temperature (1100 °C) oxidation of B doped MoSi2 in synthetic air has been investigated. A (boro)silicate layer is formed on the surface of the alloy, which features a mixture of amorphous SiO2 and cristobalite. After an initial transient period, the oxidation kinetics follows a parabolic growth rate law. The growth rate constant of the oxide layer is enhanced by the boron in the alloy by 90 % per at.% B. The increase in growth rate is associated with boron mitigating the formation of cristobalite thereby promoting the formation of amorphous SiO2., Team Marcel Hermans, Team Vera Popovich, Team Joris Dik

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 Ti2NiOx 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., Team Vera Popovich, Team Marcel Hermans

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 Ti2NiOx 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., Team Vera Popovich, QN/Afdelingsbureau, Team Maria Santofimia Navarro, Team Marcel Hermans

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.], Team Arjan Mol, Team Vera Popovich, Team Yaiza Gonzalez Garcia

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., Team Vera Popovich, Team Marcel Sluiter, QN/Afdelingsbureau, Team Amarante Bottger, Team Marcel Hermans

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., Team Arjan Mol, Team Vera Popovich, Team Yaiza Gonzalez Garcia

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., Team Vera Popovich, Team Marcel Hermans, Transport Engineering and Logistics

Additively manufactured (AM) biodegradable magnesium (Mg) scaffolds with precisely controlled and fully interconnected porous structures offer unprecedented potential as temporary bone substitutes and for bone regeneration in critical-sized bone defects. However, current attempts to apply AM techniques, mainly powder bed fusion AM, for the preparation of Mg scaffolds, have encountered some crucial difficulties related to safety in AM operations and severe oxidation during AM processes. To avoid these difficulties, extrusion-based 3D printing has been recently developed to prepare porous Mg scaffolds with highly interconnected structures. However, limited bioactivity and a too high rate of biodegradation remain the major challenges that need to be addressed. Here, we present a new generation of extrusion-based 3D printed porous Mg scaffolds that are coated with MgF2 and MgF2-CaP to improve their corrosion resistance and biocompatibility, thereby bringing the AM scaffolds closer to meeting the clinical requirements for bone substitutes. The mechanical properties, in vitro biodegradation behavior, electrochemical response, and biocompatibility of the 3D printed Mg scaffolds with a macroporosity of 55% and a strut density of 92% were evaluated. Furthermore, comparisons were made between the bare scaffolds and the scaffolds with coatings. The coating not only covered the struts but also infiltrated the struts through micropores, resulting in decreases in both macro- and micro-porosity. The bare Mg scaffolds exhibited poor corrosion resistance due to the highly interconnected porous structure, while the MgF2-CaP coatings remarkably improved the corrosion resistance, lowering the biodegradation rate of the scaffolds down to 0.2 mm y-1. The compressive mechanical properties of the bare and coated Mg scaffolds before and during in vitro immersion tests for up to 7 days were both in the range of the values reported for the trabecular bone. Moreover, direct culture of MC3T3, Biomaterials & Tissue Biomechanics, Team Peyman Taheri, Team Arjan Mol, Team Vera Popovich

This study investigates the feasibility of in-situ manufacturing of a functionally graded metallic-regolith. To fabricate the gradient, digital light processing, an additive manufacturing technique, and spark plasma sintering were selected due to their compatibility with metallic-ceramic processing in a space environment. The chosen methods were first assessed for their ability to effectively consolidate regolith alone, before progressing to sintering regolith directly onto metallic substrates. Optimized processing conditions based on the sintering temperature, initial powder particle size, and different compositions of the lunar regolith powders were identified. Experiments have successfully proven the consolidation of lunar regolith simulants at 1050°C under 80 MPa with digital light processing and spark plasma sintering, while the metallic powders can be fully densified at relatively low temperatures and a pressure of 50 MPa with spark plasma sintering. Furthermore, the lunar regolith and Ti 6 Al 4 V gradient was proven to be the most promising combination. While the current study showed that it is feasible to manufacture a functionally graded metallic-regolith, further developments of a fully optimized method have the potential to produce tailored, high-performance materials in an off-earth manufacturing setting for the production of aerospace, robotic, or architectural components., Team Vera Popovich, Team Marcel Hermans

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 (El) 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., Team Vera Popovich, Team Marcel Hermans

Additively manufactured (AM) biodegradable magnesium (Mg) scaffolds with precisely controlled and fully interconnected porous structures offer unprecedented potential as temporary bone substitutes and for bone regeneration in critical-sized bone defects. However, current attempts to apply AM techniques, mainly powder bed fusion AM, for the preparation of Mg scaffolds, have encountered some crucial difficulties related to safety in AM operations and severe oxidation during AM processes. To avoid these difficulties, extrusion-based 3D printing has been recently developed to prepare porous Mg scaffolds with highly interconnected structures. However, limited bioactivity and a too high rate of biodegradation remain the major challenges that need to be addressed. Here, we present a new generation of extrusion-based 3D printed porous Mg scaffolds that are coated with MgF2 and MgF2-CaP to improve their corrosion resistance and biocompatibility, thereby bringing the AM scaffolds closer to meeting the clinical requirements for bone substitutes. The mechanical properties, in vitro biodegradation behavior, electrochemical response, and biocompatibility of the 3D printed Mg scaffolds with a macroporosity of 55% and a strut density of 92% were evaluated. Furthermore, comparisons were made between the bare scaffolds and the scaffolds with coatings. The coating not only covered the struts but also infiltrated the struts through micropores, resulting in decreases in both macro- and micro-porosity. The bare Mg scaffolds exhibited poor corrosion resistance due to the highly interconnected porous structure, while the MgF2-CaP coatings remarkably improved the corrosion resistance, lowering the biodegradation rate of the scaffolds down to 0.2 mm y-1. The compressive mechanical properties of the bare and coated Mg scaffolds before and during in vitro immersion tests for up to 7 days were both in the range of the values reported for the trabecular bone. Moreover, direct culture of MC3T3, Biomaterials & Tissue Biomechanics, Team Peyman Taheri, Team Arjan Mol, Team Vera Popovich

This study investigates the feasibility of in-situ manufacturing of a functionally graded metallic-regolith. To fabricate the gradient, digital light processing, an additive manufacturing technique, and spark plasma sintering were selected due to their compatibility with metallic-ceramic processing in a space environment. The chosen methods were first assessed for their ability to effectively consolidate regolith alone, before progressing to sintering regolith directly onto metallic substrates. Optimized processing conditions based on the sintering temperature, initial powder particle size, and different compositions of the lunar regolith powders were identified. Experiments have successfully proven the consolidation of lunar regolith simulants at 1050°C under 80 MPa with digital light processing and spark plasma sintering, while the metallic powders can be fully densified at relatively low temperatures and a pressure of 50 MPa with spark plasma sintering. Furthermore, the lunar regolith and Ti 6 Al 4 V gradient was proven to be the most promising combination. While the current study showed that it is feasible to manufacture a functionally graded metallic-regolith, further developments of a fully optimized method have the potential to produce tailored, high-performance materials in an off-earth manufacturing setting for the production of aerospace, robotic, or architectural components., Team Vera Popovich, Team Marcel Hermans

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 (El) 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., Team Vera Popovich, Team Marcel Hermans

In this paper, laser powder-bed fusion (L-PBF) additive manufacturing (AM) with a high-temperature inductive platform preheating was used to fabricate intermetallic TiAl-alloy samples. The gas atomized (GA) and mechanically alloyed plasma spheroidized (MAPS) powders of the Ti-48Al-2Cr-2Nb (at. %) alloy were used as the feedstock material. The effects of L-PBF process parameters-platform preheating temperature-on the relative density, microstructure, phase composition, andmechanicalproperties ofprintedmaterialwere evaluated. Crack-free intermetallic samples with a high relative density of 99.9% were fabricated using 900 °C preheating temperature. Scanning electron microscopy and X-Ray diffraction analyses revealed a very fine microstructure consisting of lamellar α2/γ colonies, equiaxed γ grains, and retained β phase. Compressive tests showed superior properties of AM material as compared to the conventional TiAl-alloy. However, increased oxygen content was detected inMAPS powder compared to GA powder (~1.1 wt. % and ~0.1 wt. %, respectively), which resulted in lower compressive strength and strain, but higher microhardness compared to the samples produced from GA powder., (OLD) MSE-5

Additive Manufacturing (AM) is an attractive way of producing parts of intermetallic titanium alloys. However, high brittleness of these alloys makes it challenging to produce crack-free intermetallic parts by AM. One way to overcome this problem is to use high-temperature powder-bed preheating. In this paper, Ti-48Al-2Cr-2Nb alloy was obtained by selective laser melting process with high-temperature preheating of 800-900 ºC. Crack-free specimens with a relative density of 99.9% were fabricated using an optimized process parameter set. Microstructure and phase composition were studied using scanning electron microscopy and X-Ray diffraction to reveal a fine microstructure consisting of lamellar a2/? colonies, equiaxed ? grains, and retained ß phase. Compressive tests and microhardness measurements showed that the produced alloy exhibited superior properties compared to the conventionally obtained TiAl-alloy., (OLD) MSE-5

Additive Manufacturing (AM) is an attractive way of producing parts of intermetallic titanium alloys. However, high brittleness of these alloys makes it challenging to produce crack-free intermetallic parts by AM. One way to overcome this problem is to use high-temperature powder-bed preheating. In this paper, Ti-48Al-2Cr-2Nb alloy was obtained by selective laser melting process with high-temperature preheating of 800-900 ºC. Crack-free specimens with a relative density of 99.9% were fabricated using an optimized process parameter set. Microstructure and phase composition were studied using scanning electron microscopy and X-Ray diffraction to reveal a fine microstructure consisting of lamellar a2/? colonies, equiaxed ? grains, and retained ß phase. Compressive tests and microhardness measurements showed that the produced alloy exhibited superior properties compared to the conventionally obtained TiAl-alloy., (OLD) MSE-5