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Additive Manufacturing of NiTiHf HTSMA
Additive Manufacturing of NiTiHf HTSMA
Scripta Materialia
Regular article
a r t i c l e i n f o a b s t r a c t
Article history: A NiTi-20Hf high temperature shape memory alloy (HTSMA) was additively manufactured by selective laser
Received 11 September 2017 melting (SLM) technique using NiTiHf powder. The thermomechanical and shape memory response were com-
Received in revised form 12 October 2017 pared to the conventional vacuum induction skull melted counterpart. Transformation temperatures of the SLM
Accepted 12 October 2017
material were found to be above 200 °C and slightly lower due to the additional oxygen pick up from the gas at-
Available online 5 November 2017
omization and melting process. The shape memory response in compression was measured for stresses up to
Keywords:
500 MPa, and transformation strains were found to be very comparable (up to 1.26% for as-extruded; up to
NiTiHf 1.52% for SLM).
High temperature shape memory alloys © 2017 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.
Additive manufacturing
Actuators
Commercially available NiTi shape memory alloys (SMAs) present Up to now, different techniques have been used to process NiTiHf in-
transformation temperatures (TTs) below 100 °C enabling their practi- cluding vacuum induction melting (VIM), vacuum arc melting (VAM),
cal applications for the many technological applications requiring low cold crucible levitation melting (CCLM), copper boat induction melting
operating temperatures, such as biomedical implants and actuators (CBIM), electron beam melting (EBM), and plasma arc melting (PAM)
[1–3]. In recent years, NiTi-based high temperature shape memory al- [3,22–26]. It is well known that the processing and machining NiTi-
loys (HTSMAs) have been introduced via substitution of Ni or Ti by a based alloys, including NiTiHf, is a quite difficult task due to the high re-
third element such as Hf, Zr, Pt, Pd, and Au [4–13]. NiTi-based HTSMAs activity of the alloy, stress induced martensite, spring back effects, work
are designed to operate at temperatures above 100 °C which particular- hardening, burr formation and adhesion [27–30]. These altogether have
ly enable their applications in aerospace, automotive, oil, and many limited the geometry of NiTiHf components to sheets, strips, wires,
other industries. Among the ternary elements, Hf has attracted much at- tubes, or bars. Additive manufacturing (AM) techniques opens up possi-
tention due to its high influence on the TTs as well as its relatively low bilities to circumvent challenges in conventional manufacturing [30–
cost [14–16]. 32]. In AM techniques, the final component is being fabricated from a
It is well documented that the TTs of NiTiHf are highly dependent on virtually-sliced CAD model which enables the production of complex
its composition [17]. That being said, up to 10 at.% Hf does not have geometries (e.g., lattice-like, truss-based, curved holes, engineered po-
much influence on the TTs, while Hf concentration higher than 10 at.% rosity, hollow parts) [33,34]. Despite its high potential, no work has
linearly increase the TTs of (Ti + Hf)-rich NiTiHf, reaching 525 °C by been performed on the AM of NiTiHf in literature. To successfully
30 at.% Hf addition at the expense of Ti [3,18]. In slightly Ni-rich compo- fabricate a new material (i.e., NiTiHf), the processing parameters (e.g.,
sitions, the TTs drop at a rate of 10–15 °C per 0.1 at.% Ni [19]. However, scanning velocity, laser power and focusing, hatch spacing, and layer
the TTs drop can be compensated through appropriate post heat treat- thickness) must be optimized. It is worth noting that the thermo-
ments [20,21]. Although the ternary element addition, such as Hf, is mechanical features of NiTiHf add to the complexity of fabrication. In
known to increase the TTs, when compared to NiTi, the Ti-rich version this paper, a Ti-rich NiTiHf alloy was processed for the first time via se-
adversely affect some other features and result in relatively low ductil- lective laser melting (SLM), the most common AM technique for pow-
ity, a low strength, a large temperature hysteresis (N 50 °C), a low resis- der metals. In addition, the mechanical and thermomechanical
tance to slip, and a lack of cyclic stability [18]. features of SLM NiTiHf compared to conventionally processed alloy
were investigated.
A slightly Ti-rich Ni49.8Ti30.2Hf20 (at.% of measured composition)
⁎ Corresponding author. alloy was produced by vacuum induction skull melting process. Part of
E-mail address: mohammad.elahinia@utoledo.edu (M. Elahinia). the cast ingots were vacuum homogenized at 1050 °C for 72 h, followed
https://doi.org/10.1016/j.scriptamat.2017.10.016
1359-6462/© 2017 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.
M. Elahinia et al. / Scripta Materialia 145 (2018) 90–94 91
Table 1
ICP values obtained for as-extruded, powder, and SLM NiTiHf components.
by hot extrusion at 900 °C (alloy designated as-extruded). Hot extrusion the basic microstructure of the alloys, the samples were mounted,
was aimed to improve the transformation strain levels, cyclic stability, polished, etched, and imaged in a JEOL 840 SEM. Differential scanning
and two-way shape memory effect (TWSME) of as-cast NiTiHf alloy calorimetry (DSC) analyses were conducted using a TA Instruments
[2]. Other ingots were subjected to an Electrode induction-melting gas Q1000 with heating/cooling rate of 10 °C/min. Each specimen was cy-
atomization (EIGA) by TLS Technik GmbH (Bitterfield, Germany) to pro- cled 10 times between 0 and 370 °C to evaluate the stability of the
duce the powder. EIGA is a unique technique that produces spherical phase transformation temperatures. Martensite start (Ms) and martens-
powders with extremely low impurity (e.g., oxygen, carbon, ceramic ite finish (Mf) temperatures on cooling and austenite start (As) and aus-
impurities, nitrogen) contents. A range of 25–75 μm particle fractions tenite finish (Af) temperatures on heating were determined by tangent
was used to ensure a good compromise of layer resolution and technique. Thermomechanical tests of both as-extruded and SLM fabri-
flowability. A SLM machine (Phenix Systems PXM) was used to produce cated samples were conducted using an MTS® 810 servo-hydraulic load
NiTiHf components directly from powder. The Phenix Systems PXM is a frame equipped with an Ameritherm NovaStar 7 kW induction heating
powder-bed based SLM machine equipped with a 300 W Ytterbium system. A Eurotherm controller was used to control the test tempera-
fiber laser manufactured by JK Lasers. The laser beam was directly fo- ture with type-K thermocouples, spot-welded directly to the middle of
cused via galvanometric mirrors producing a beam diameter of approx- the sample gage length. A heating rate of 20 °C/min was used while
imately 80 μm, a beam quality of M2 b 1.2, and a collimated (TEM00) cooling was partially controlled. Strains were measured from the dis-
beam with a Gaussian profile [35,36]. Prior to the fabrication, a CAD soft- placement of the platen surfaces using a Micro-Epsilon™ optoControl
ware and a Phenix Systems software were used to create the 3D model 2600, non-contacting LED based micrometer. Constant-force thermal
and to slice it into the requisite layers, respectively. In PXM machine, a cycling was performed in compression at stresses ranging from 0 to
feeding piston moves upward to provide the powder. Subsequently, a 500 MPa. One SLM rectangular cube component with dimensions of
metal scraper and a metal roller collect, deposit, and compact the pow- 2 mm × 2 mm × 5 mm, fabricated in the horizontal direction was tested
der layer on the building platform. Then, a laser selectively melts and under a minimum stress of 30 MPa due to the small sample size. The ex-
binds the powder particles to each other. Finally, the building piston truded rods with a diameter of 5 mm and 10 mm long were tested
drops down with a layer thickness to accommodate the next layer. starting at 0 MPa. Then, each sample was cycled between 50 °C and
This procedure is repeated until the fabrication of the fully dense com- 450 °C at a rate of 20 °C/min in 100 MPa increments from the lowest
ponent is completed [33,37,38]. The fabrication procedure was conduct- stress to 500 MPa. Finally, each sample was tested at “0 MPa” to inves-
ed under argon atmosphere which decreased the oxygen level to tigate their two-way shape memory.
500 ppm. The SLM processing Parameters used in fabricating NiTiHf Table 1 shows the ICP results comparing the compositions of pow-
components were considered to be 250 W laser power, 30 μm layer der, as-extruded, and SLM NiTiHf. When compared to as-extruded ma-
thickness, 1.25 m/s scanning velocity, and 120 μm hatch spacing. terial, the level of Ni-loss are reported to be 0.03 at.% and 0.21 at.% for
Chemical compositions of the as-extruded, powder, and SLM NiTiHf the powder and SLM material, respectively. It can be inferred that the
were quantitatively evaluated using inductively coupled plasma atomic SLM process more influence the Ni content rather than the powder
emission spectroscopy (ICP-AES) for metallic elements and the LECO® preparation procedure. Ni loss associated with SLM mostly can be at-
determinators for oxygen, nitrogen sand carbon content. To determine tributed to the fact that Ni element tend to evaporate sooner than the
Fig. 1. (a) SEM image of Powder, (b) particle distribution, (c) optical and (d) SEM images of SLM NiTiHf.
92 M. Elahinia et al. / Scripta Materialia 145 (2018) 90–94
Fig. 3. Constant-force thermal cycling of the Ni49.8Ti30.2Hf20 alloy under compression: (a) as-extruded and (b) SLM. The red and blue curves indicate heating and cooling cycles,
respectively.
M. Elahinia et al. / Scripta Materialia 145 (2018) 90–94 93
Fig. 4. (a) The transformation temperatures, (b) transformation strain and (c) irrecoverable strain vs. applied stress of Ni49.8Ti30.2Hf20 in the as-extruded (Note: dotted lines) and SLM (solid
lines) samples.
increases from 43.7 to 61.7 °C for as-extruded and from 45.6 to 80.6 °C material. This is likely attributed to the formation of secondary Ti-rich
for SLM material with increasing stress from 0 to 500 MPa. Fig. 4b dem- phases during atomization and SLM technique. The microstructural
onstrates transformation strain at each cycle for both as-extruded and analysis confirms the existence of Ti-rich secondary phases. The con-
SLM NiTiHf alloys. At elevated levels of stress (100–500 MPa), a greater stant-force thermal cycling response of SLM material demonstrated
net shape change is observed for SLM material compared to as-extrud- higher transformation strains, but identical trend, with as-extruded ma-
ed. The transformation strain increased from 0.24% to 1.26% for the as- terial. Finally, the stress-free thermal cycling responses of both SLM and
extruded and from 0.24% to 1.52% for SLM when the applied stress as-extruded material exhibited small magnitudes of two-way shape
was increased from 100 to 500 MPa, respectively. Higher stress levels memory. The microstructure and laser optimization will be a subject
are able to reorient more of the martensite twins in an orientation of our future activity. Further, before transition into more complex
that favor the applied strain during reverse transformation, which result shapes, this material will be further evaluated and examined in tension
in the availability of more strain to be recovered during the forward and/or torsion to find out the effect of inclusions and cracks on the func-
transformation. In general, there exists a critical point for each alloy tional response and durability.
where this reorientation effect is maximized, however, the existence
of high internal and external stresses does not allow for fully recovery.
Therefore, starting from the critical point, the transformation strains Acknowledgements
start to decrease [41]. It is clear that the critical point is not in the
range of selected applied stress for this study. Finally, Fig. 4c demon- Funding support from the NASA Glenn Research Center, Transforma-
strates that the irrecoverable strain increase with higher level of applied tional Tools & Technologies (TTT) Project is gratefully acknowledged
stress for both cases. It can be observed that the irrecoverable strains of (contract #NNC16VA75P).
two materials are essentially identical.
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