1 s2.0 S2772369024000252 Main
1 s2.0 S2772369024000252 Main
1 s2.0 S2772369024000252 Main
Short Communication
A R T I C L E I N F O A B S T R A C T
Keywords: Additive manufacturing has revolutionized the creation of complex and intrinsic structures, offering tailored
Shape memory alloys designs for enhanced product performance across various applications. Architected cellular or lattice structures
Functional performance exemplify this innovation, customizable for specific mechanical or functional requirements, boasting advantages
Architected metamaterials
such as reduced mass, heightened load-bearing capabilities, and superior energy absorption. Nonetheless, their
Additive manufacturing
Laser Powder Bed Fusion
single-use limitation arises from plastic deformation resulting from localized yield damage or plastic buckling.
Incorporating NiTi shape memory alloys (SMAs) presents a solution, enabling structures to recover their original
shape post-unloading. In this study, an NiTi architected metastructure, featuring auxetic behavior and a negative
Poisson’s ratio, was designed and fabricated via laser powder bed fusion (LPBF). The samples exhibit promising
superelastic performance with recoverable deformation strains at room temperature. Comprehensive charac
terization processes evaluated the functional performance of the fabricated metastructures. The metastructure
geometry promoted microstructure formation primarily along the wall thickness. Cycling compression tests,
conducted at three applied force levels, demonstrated stable cyclic behavior with up to 3.8 % reversible
deformation strain, devoid of plastic buckling or yielding damage. Furthermore, the NiTi metastructures dis
played robust energy absorption capacity and damping behavior, underscoring their potential for reusable en
ergy dissipators in various industries including aerospace, automotive, construction, and etc.
* Corresponding author.
E-mail address: [email protected] (M. Mehrpouya).
https://doi.org/10.1016/j.addlet.2024.100216
Received 11 February 2024; Received in revised form 20 April 2024; Accepted 22 April 2024
Available online 23 April 2024
2772-3690/© 2024 The Author(s). Published by Elsevier B.V. This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/).
C.A. Biffi et al. Additive Manufacturing Letters 10 (2024) 100216
2
C.A. Biffi et al. Additive Manufacturing Letters 10 (2024) 100216
Fig. 2. The optical microscopy images of the NiTi lattices show the quality of the sample fabrication by the LPBF technique on the node (a) and on the edge (b).
2.2. Material and fabrication and a total of 3000 images were acquired for the examination. The ob
tained tomography datasets were reconstructed using Dragonfly soft
NiTi samples were produced utilizing an LPBF system (Renishaw, ware (Comet Technologies Canada Inc), and the 3D distribution of
AM400, UK) employing Ni56Ti46 (wt.%) spherical powder (Nanoval, deformation or damage in the samples was determined using Dragon
Germany), having a mesh distribution from 16 μm to 63 μm. The LPBF fly’s segmentation toolkit.
process parameters outlined in Table 1 were chosen for the fabrication of
the NiTi architected structures. The adopted LPBF system was equipped
with a pulsed wave laser, and the pulse duration, rather than scanning 2.4. Microstructural characterization
speed, was utilized to define the appropriate process conditions for
achieving the desired NiTi properties [19,35]. The samples were The martensitic transformation temperatures were detected through
extracted from the platform using a wire electrical discharge cutting differential scanning calorimetry (DSC, model Q25 from TA Instrument,
machine. To enhance the functional characteristics of the printed USA), carried out with a heating/cooling scan rate of 10 ◦ C/min, within
specimens, we applied a specific low-temperature heat treatment pro a temperature range from − 100 ◦ C up to 100 ◦ C. Initial NiTi powder, as
cess. This process primarily aims to release the residual stresses induced built and heat treated samples were analyzed through DSC.
by the LPBF process. As a result, the as-built samples underwent Diffraction data (CuKα, λ=1.5418 Å) were collected on a θ:θ vertical
annealing at 500 ◦ C for 5 min, followed by water quenching. scan P analytical X’Pert PRO diffractometer, equipped with parallel
(Soller) slits – 0.04 rad – and a real-time multiple strip detector. The
generator was operated at 40 kV and 30 mA; slits were used with a
2.3. 2D and 3D visual characterization divergence of 0.5◦ The scans were performed in the 10–120◦ 2θ range at
25 ◦ C. Phase identification was carried out on the heat treated NiTi
Optical microscopy images were captured using a Digital Microscope sample.
(Keyence, VHX-7000 N, Belgium) for surface investigation of the NiTi Scanning electron microscopy (SEM) was applied for additional ex
lattice samples. A selected sample was subjected to X-ray micro amination, employing a Thermo Fisher (Model Phenom XL) and JEOL
–Computed Tomography (µ-CT) for detailed qualification. The µ-CT was (Model JSM-7200F) equipped with EDS and electron backscatter
performed using GE equipment (model V, TOMEX), featuring a screen diffraction (EBSD) detectors to thoroughly analyze and characterize the
DXR-250 with a pixel size of 2000 × 2000 | 200 μm. The acquisition microstructure. Image acquisition was conducted using a back-scattered
parameters were set as follows: power=13 W, spatial resolution= 14 µm, electron (BSE) detector to offer a comprehensive depiction of various
Fig. 3. Micro-CT analysis of the built NiTi architecture sample: xy view (a) and 3D visualization (b).
3
C.A. Biffi et al. Additive Manufacturing Letters 10 (2024) 100216
Fig. 4. The trend of the wall thickness of the sample with its statistical analysis.
phases present in the microstructure. To enhance image quality and tests at three levels of force (4–8–12 kN), and each test was repeated
mitigate charging issues during EBSD imaging, specific samples were three times to ensure accuracy and reliability.
embedded in conductive epoxy.
3. Results and discussion
2.5. Mechanical characterization
3.1. Visual investigation of NiTi structures
The mechanical behavior of the NiTi architected structures was
The NiTi structures were successfully printed following the experi
investigated through a cyclic compression test, conducted with 10 cycles
mental plan outlined in the previous section. As depicted in Fig. 2, the
of loading and unloading to ensure stable mechanical responses for each
printed NiTi lattice exhibits a defect-free surface with no discernible
sample. The tests were performed at room temperature, 25 ◦ C, (using a
cracks. The scanning strategy employed during printing, comprising
tensile test machine (Zwick, model Z100, Germany) equipped with a
meander patterns consisting of contour and hatch paths, is visible on the
100 kN load cell. A constant speed of 0.5 mm/min was maintained for all
Fig. 5. DSC scans of the initial powder, as built and heat-treated NiTi samples.
4
C.A. Biffi et al. Additive Manufacturing Letters 10 (2024) 100216
Table 2
Transformation Temperatures (TT) of the initial powder, as built and heat-treated NiTi samples. All temperature units are ◦ C.
TT As Ap Af Rs Rp Rf Ms Mp Mf
upper surfaces. The choice of the meander strategy, splitted in hatch and
contour, depends on the significant thickness of the architected struc
ture. Previous works were carried out on the printing of NiTi thinner
lattice samples, requiring the adjustment of the principal process pa
rameters for implementing a different scanning strategy, namely lattice
[19]. Additionally, linear laser scans were used in the central part of the
samples, while the border was created using concentric lines.
To evaluate the inner quality of the fabricated structures, a µ-CT scan
was performed. The 3D reconstruction in Fig. 3 illustrates the defects’
size through a color scale representation. Notably, the nodes of the
lattice structure exhibit relatively more defects, with an average size of
approximately 100 µm. Also visible are cracks due to the compression
testing. Despite the presence of some defects, the volume fraction was
measured as 0.07% and this is well within the normal range for an
additively manufactured material.
From the µ-CT scans, a wall thickness evaluation could be made.
Fig. 4 shows that the wall thickness ranged mainly around 1 mm (shown
in yellow) with some thicker regions at the junctions (shown in red). The
statistical thickness distribution is included. Fig. 6. XRD diffractogram of the heat-treated NiTi sample.
3.2. Microstructural analysis of NiTi structures was carried out during the LPBF process.
Fig. 6 shows the XRD spectrum that was carried out on the heat-
The microstructure of the NiTi samples was analyzed through DSC, treated sample at room temperature. Austenite (cubic structure, B2)
XRD, and EBSD tests to obtain a complete overview in terms of trans was predominantly detected in the NiTi sample, consistent with the
formation temperatures of the martensitic transformation, phase iden Austenite Finish (Af) temperature measured from the DSC scans. The
tification, and distribution inside the architectural samples. sample exhibited a preferential crystallographic orientation, influenced
Initially, the transformation temperatures (TTs) of the initial pow by the rapid laser motion on the powder bed and the subsequent rapid
der, as-built, and heat-treated samples were measured via DSC. Due to solidification. The most intense diffraction reflection was associated
the significant sensitivity of the performances in NiTi SMAs with respect with the (110) peak. Epitaxial growth and columnar grain growth
to the chemical composition, it was decided to proceed with a controlled the solidification, attributed to the very high cooling rates
comparative analysis of the TTs from the feedstock material through the characteristic of LPBF.
LPBF process to the post-treated sample. Further microstructural Additionally, minor peaks associated with the B19′ phase
investigation would focus only on the heat-treated samples. (martensite) were observed. These minor peaks were expected, given
Fig. 5 presents the DSC test results for the initial NiTi powder, as- that the patterns were collected at room temperature, very close to Af.
built, and heat-treated architected structures. The NiTi powder exhibi For a more in-depth understanding of the microstructure, EBSD analysis
ted a multistage martensitic transformation (MT) upon heating and was conducted.
cooling due to compositional inhomogeneities and residual stresses The EBSD analysis provides a comprehensive insight into the grain
arising from the gas atomization process [36]. In contrast, the as-built formation of the 3D printed samples across various sections of the
structure displayed a single-stage MT upon heating and a double-stage structure. Fig. 7 illustrates the outcomes of the EBSD test conducted on
MT upon cooling, with the two peaks largely overlapping each other, the XZ section of the sample. Indexing is carried out based on the body-
resulting in TT values shifting to lower values. The heat treatment centered cubic austenite. Consequently, the orientation image micro
conducted at 500 ◦ C for 5 min (indicated as HT 500) promoted a sharper graphs (OIM) are computed for the normal direction of the section,
peak upon heating, indicating the martensite-to-austenite trans along with the inverse pole figures (IPF) in the Z, Y, and X directions.
formation. Additionally, two well-defined peaks were observed during As depicted, there are non-indexed areas represented in black, sug
cooling. The first peak corresponded to the transformation from gesting a potential association with localized martensite regions, as re
austenite to R-phase, distinguished by limited thermal hysteresis be ported in other work in the literature [17]. However, most of the
tween the peaks upon heating and cooling. The second peak was related analyzed surfaces exhibited the presence of austenite, which is in good
to the phase transformation from R-phase to martensite. agreement with the XRD (Fig. 6) and DSC (Fig. 5) analyses. Similar re
Table 2 presents the values of TTs, obtained from the DSC scans sults were achieved in the literature [37,38]. The results further reveal a
shown in Fig. 5. This includes the evaluation of austenite start (As), peak lack of uniform texture, with the latter manifesting as a more reddish
(Ap), and finish (Af), R-phase start (Rs), peak (Rp), and finish (Rf), as center and displaying random colors in the OIM. The specimen exhibited
well as martensite start (Ms), peak (Mp), and finish (Mf) temperatures, elongated grains in the building direction (see Fig. 7), while the shape of
respectively. the typical liquid pools is not detectable. On the contrary, columnar
In conclusion, the NiTi powder shows wide and partially overlapped grains can be observed in Fig. 7, growing orthogonally to the platform,
peaks of the MT; the corresponding values of TTs confirmed a complete as confirmed by other works in the literature [35].
phase transformation in austenite at room temperature, promoting a Fig. 8 presents the results of the EBSD analysis conducted on the XY
superelastic behavior. The TTs of the as-built structure, ranged in a section of the NiTi samples. In these images, epitaxial grains with di
similar temperature interval of the power, meaning no significant Ni loss mensions significantly smaller than those in the XZ view (refer to Fig. 7)
5
C.A. Biffi et al. Additive Manufacturing Letters 10 (2024) 100216
Fig. 7. EBSD analysis of the XZ section in the NiTi structure, depicted using orientation image micrographs (OIM). The visuals correspond to (a) Band Contrast (BC)
and (b-d) inverse pole figures (IPF) in the Z, Y, and X directions, respectively.
Fig. 8. EBSD findings on the XY section of the NiTi structure, illustrated through orientation image micrographs (OIM). The images correspond to (a) Band Contrast
(BC) and (b-d) inverse pole figures (IPF) in the Z, Y, and X directions, respectively.
6
C.A. Biffi et al. Additive Manufacturing Letters 10 (2024) 100216
7
C.A. Biffi et al. Additive Manufacturing Letters 10 (2024) 100216
Fig. 11. Summary of compression testing results, showing the total displacement and the recoverable deformation ratio of the NiTi architected structures when
compressed to 4 kN, 8 kN, and 12 kN.
Fig. 12. Dissipated energy and specific dissipation energy values for the NiTi lattice samples were compressed to 4 kN, 8 kN, and 12 kN.
specific energy dissipation values of 0.0821 kN.mm/gr, 0.2802 kN.mm/ an applied force of up to 12 kN. This underscores the capability of
gr, and 0.7747 kN.mm/gr for the respective loads of 4 kN, 8 kN, and 12 this design to enhance the functional performance and deformability
kN. of the structure, making it highly suitable for versatile and adaptive
applications.
4. Conclusion
The combination of superelasticity, high deformation capacity, and
This study investigated the mechanical performance of 3D printed efficient energy dissipation showcased in this study holds significant
NiTi architected metamaterials. The fabricated samples showcased a implications for various engineering fields, such as aerospace, robotics,
remarkable superelastic response emphasizing their potential for diverse and medical devices. These findings provide a solid foundation for
and adaptable applications. Moreover, these samples displayed an further advancements in the design and optimization of 3D printed NiTi
excellent capacity for energy dissipation and damping behavior, architected metamaterials, opening new avenues for materials engi
underscoring their efficiency in dissipating mechanical energy. The neering and enhanced performance in engineered systems.
outcomes of this research are summarized as follows:
CRediT authorship contribution statement
• The designed auxetic meta-structures were successfully fabricated
using an LPBF printing setup and tested using a wide range of C.A. Biffi: Writing – review & editing, Resources, Investigation,
characterization methods. The use of µ-CT scanning allowed us to Formal analysis. C. Soyarslan: Writing – review & editing, Software,
evaluate the relative density of the lattice structures, which was Formal analysis, Conceptualization. J. Fiocchi: Investigation, Formal
found to be as high as 99.85 %, signifying excellent overall structural analysis. C. Bregoli: Investigation, Formal analysis. A. du Plessis:
integrity. Writing – review & editing, Investigation, Formal analysis. A. Tuissi:
• Low-temperature heat treatment, carried out at 500 ◦ C for 5 min, was Visualization, Investigation. M. Mehrpouya: Writing – original draft,
successfully performed to promote the superelastic properties of the Supervision, Methodology, Investigation, Formal analysis,
3D printed NiTi samples. The results showed that the martensitic Conceptualization.
transformation was set in a temperature range suitable to obtain the
austenitic phase.
Declaration of competing interest
• The fabricated NiTi metamaterials demonstrated significant recov
erable deformation strains ranging from 1.5 to 3.8 %, achieved under
The authors declare the following financial interests/personal
8
C.A. Biffi et al. Additive Manufacturing Letters 10 (2024) 100216
relationships which may be considered as potential competing interests: [13] A. du Plessis, et al., Properties and applications of additively manufactured
metallic cellular materials: a review, Prog Mater Sci (2021) 100918.
One of the authors of this article is part of the Editorial Board of the
[14] F. Yazdandoost, et al., Energy dissipation of shock-generated stress waves through
journal. To avoid potential conflicts of interest, the responsibility for the phase transformation and plastic deformation in NiTi alloys, Mech. Mater. 137
editorial and peer-review process of this article lies with the journal’s (2019) 103090.
other editors. Furthermore, the authors of this article were removed [15] D. Kim, et al., 3D and 4D Printing of Complex Structures of Fe Mn Si-Based Shape
Memory Alloy Using Laser Powder Bed Fusion, Adv. Mater Interfaces 9 (13) (2022)
from the peer review process and had no and will not have any access to 2200171.
confidential information related to the editorial process of this article. [16] R. Xi, et al., Effect of Fe addition on the microstructure, transformation behaviour
and superelasticity of NiTi alloys fabricated by laser powder bed fusion, Virtual
Phys. Prototyp. 18 (1) (2023) e2126376.
Data availability [17] S. Khademzadeh, Precision additive manufacturing of NiTi shape memory parts
using micro-laser powder bed fusion, Progr. Addit. Manuf. (2021) 1–14.
Data will be made available on request. [18] T. Gustmann, et al., Properties of a superelastic NiTi shape memory alloy using
laser powder bed fusion and adaptive scanning strategies, Progre. Addit. Manuf. 5
(2020) 11–18.
[19] C.A. Biffi, et al., Microstructural and mechanical response of NiTi lattice 3D
Acknowledgements structure produced by selective laser melting, Metals (Basel) 10 (6) (2020) 814.
[20] S. Bernard, et al., Compression fatigue behavior of laser processed porous NiTi
alloy, J. Mech. Behav. Biomed. Mater. 13 (2012) 62–68.
The authors express their gratitude to Nicola Bennato for his support [21] M.T. Andani, et al., Mechanical and shape memory properties of porous Ni50.
in the 3D printing process. Also, we would like to appreciate the support 1Ti49. 9 alloys manufactured by selective laser melting, J. Mech. Behav. Biomed.
Mater. 68 (2017) 224–231.
of Mr. Nick Helthuis and Mr. Bert Vos for their valuable assistance in
[22] S. Dadbakhsh, et al., Laser additive manufacturing of bulk and porous shape-
setting up the microstructure and mechanical testing procedures. memory NiTi alloys: from processes to potential biomedical applications, MRS
Bulletin 41 (10) (2016) 765–774.
References [23] W. Chen, et al., Compressive mechanical properties and shape memory effect of
NiTi gradient lattice structures fabricated by laser powder bed fusion, Int. J.
Extreme Manuf. 4 (4) (2022) 045002.
[1] M. Mehrpouya, H.C. Bidsorkhi, MEMS Applications of NiTi Based Shape Memory [24] J. Sun, et al., Laser powder bed fusion of diatom frustule inspired bionic NiTi
Alloys: a Review, Micro Nanosyst 8 (2) (2016) 79–91. lattice structures: compressive behavior and shape memory effect, Smart Mater.
[2] Elahinia, M., Shape Memory Alloy Actuators: Design, Fabrication and Experimental Struct. 31 (7) (2022) 074003.
Evaluation. 2015, John Wiley & Sons. [25] Z. Yan, et al., Superelastic response and damping behavior of additively
[3] Mehrpouya, M., et al., Laser Welding of Nickel-Titanium (NiTi) Shape Memory manufactured Nitinol architectured materials, Addit. Manuf. 68 (2023) 103505.
alloys, in Advanced Welding and Deforming. 2021, Elsevier. p. 203–230. [26] Z. Yuan, Z. Cui, J. Ju, Micropolar homogenization of wavy tetra-chiral and tetra-
[4] M. Köhl, et al., Characterization of porous, net-shaped NiTi alloy regarding its achiral lattices to identify axial–shear coupling and directional negative Poisson’s
damping and energy-absorbing capacity, Mater. Sci. Eng.: A 528 (6) (2011) ratio, Mater Des. 201 (2021) 109483.
2454–2462. [27] C. Körner, Y. Liebold-Ribeiro, A systematic approach to identify cellular auxetic
[5] S. Saedi, et al., Energy Damping in Shape Memory Alloys: a Review, J. Alloys materials, Smart Mater. Struct. 24 (2) (2014) 025013.
Compd. (2023) 170286. [28] C.A. Biffi, et al., Functional performance of NiTi shape memory architected
[6] M. Benedetti, et al., Architected cellular materials: a review on their mechanical structures produced by laser powder bed fusion (LPBF), Trans. Addit. Manuf. Meets
properties towards fatigue-tolerant design and fabrication, Mater. Sci. Eng.: R: Rep. Med. 5 (S1) (2023) 821.
144 (2021) 100606. [29] A. Mauko, et al., Dynamic deformation behaviour of chiral auxetic lattices at low
[7] D. Gu, et al., Additively manufacturing-enabled hierarchical NiTi-based shape and high strain-rates, Metals (Basel) 11 (1) (2020) 52.
memory alloys with high strength and toughness, Virtual Phys. Prototyp. 16 (sup1) [30] X.-c. Zhang, et al., Dynamic crushing responses of bio-inspired re-entrant auxetic
(2021) S19–S38. honeycombs under in-plane impact loading, Mater. Today Commun. 23 (2020)
[8] L. Riva, P.S. Ginestra, E. Ceretti, Mechanical characterization and properties of 100918.
laser-based powder bed–fused lattice structures: a review, Int.. J. Adv. Manuf. [31] Y. Zhang, et al., Static and dynamic properties of a perforated metallic auxetic
Technol. 113 (2021) 649–671. metamaterial with tunable stiffness and energy absorption, Int. J. Impact Eng. 164
[9] M.K. Ravari, et al., On the effects of geometry, defects, and material asymmetry on (2022) 104193.
the mechanical response of shape memory alloy cellular lattice structures, Smart [32] B. Grünbaum, G.C. Shephard, Tilings and Patterns, Courier Dover Publications,
Mater. Struct. 25 (2) (2016) 025008. 1987.
[10] S. Afkhami, et al., Mechanical performance and design optimisation of metal [33] Dolla, W.J.S., B.A. Fricke, and B.R. Becker, Structural and drug diffusion models of
honeycombs fabricated by laser powder bed fusion, Thin-Walled Struct. 180 (2022) conventional and auxetic drug-eluting stents. 2007.
109864. [34] Y. Zhang, et al., In-plane compressive properties of assembled auxetic chiral
[11] C.W. Isaac, F. Duddeck, Recent progress in 4D printed energy-absorbing honeycomb composed of slotted wave plate, Mater. Des. 221 (2022) 110956.
metamaterials and structures, Virtual Phys. Prototyp. 18 (1) (2023) e2197436. [35] C.A. Biffi, et al., Selective laser melting of NiTi shape memory alloy: processability,
[12] A. Jafarabadi, et al., 4D printing of recoverable buckling-induced architected iron- microstructure, and superelasticity, Shape Memory Superelastic. 6 (2020)
based shape memory alloys, Mater. Des. 233 (2023) 112216. 342–353.