Scripta Materialia 145 (2018) 90–94

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Scripta Materialia

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Regular article

Additive manufacturing of NiTiHf high temperature shape memory alloy

Mohammad Elahinia a,⁎, Narges Shayesteh Moghaddam a, Amirhesam Amerinatanzi a, Soheil Saedi b,
Guher Pelin Toker b, Haluk Karaca b, Glen S. Bigelow c, Othmane Benafan c
a
Dynamic and Smart Systems Laboratory, Mechanical Industrial and Manufacturing Engineering Department, The University of Toledo, OH 43606, United States
b
Department of Mechanical Engineering, University of Kentucky, Lexington, KY 40506-0503, United States
c
NASA Glenn Research Center, Materials and Structures Division, Cleveland, OH 44135, United States

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
transformation temperatures (TTs) below 100 °C enabling their practi-
cal applications for the many technological applications requiring low
operating temperatures, such as biomedical implants and actuators
[1–3]. In recent years, NiTi-based high temperature shape memory al-
loys (HTSMAs) have been introduced via substitution of Ni or Ti by a
third element such as Hf, Zr, Pt, Pd, and Au [4–13]. NiTi-based HTSMAs
are designed to operate at temperatures above 100 °C which particular-
ly enable their applications in aerospace, automotive, oil, and many
other industries. Among the ternary elements, Hf has attracted much at-
tention due to its high influence on the TTs as well as its relatively low
cost [14–16].
It is well documented that the TTs of NiTiHf are highly dependent on
its composition [17]. That being said, up to 10 at.% Hf does not have
much influence on the TTs, while Hf concentration higher than 10 at.%
linearly increase the TTs of (Ti + Hf)-rich NiTiHf, reaching 525 °C by
30 at.% Hf addition at the expense of Ti [3,18]. In slightly Ni-rich compo-
sitions, the TTs drop at a rate of 10–15 °C per 0.1 at.% Ni [19]. However,
the TTs drop can be compensated through appropriate post heat treat-
ments [20,21]. Although the ternary element addition, such as Hf, is
known to increase the TTs, when compared to NiTi, the Ti-rich version
adversely affect some other features and result in relatively low ductil-
ity, a low strength, a large temperature hysteresis (N 50 °C), a low resis-
tance to slip, and a lack of cyclic stability [18].
⁎ Corresponding author.
E-mail address: mohammad.elahinia@utoledo.edu (M. Elahinia).
Up to now, different techniques have been used to process NiTiHf in-
cluding vacuum induction melting (VIM), vacuum arc melting (VAM),
cold crucible levitation melting (CCLM), copper boat induction melting
(CBIM), electron beam melting (EBM), and plasma arc melting (PAM)
[3,22–26]. It is well known that the processing and machining NiTi-
based alloys, including NiTiHf, is a quite difficult task due to the high re-
activity of the alloy, stress induced martensite, spring back effects, work
hardening, burr formation and adhesion [27–30]. These altogether have
limited the geometry of NiTiHf components to sheets, strips, wires,
tubes, or bars. Additive manufacturing (AM) techniques opens up possi-
bilities to circumvent challenges in conventional manufacturing [30–
32]. In AM techniques, the final component is being fabricated from a
virtually-sliced CAD model which enables the production of complex
geometries (e.g., lattice-like, truss-based, curved holes, engineered po-
rosity, hollow parts) [33,34]. Despite its high potential, no work has
been performed on the AM of NiTiHf in literature. To successfully
fabricate a new material (i.e., NiTiHf), the processing parameters (e.g.,
scanning velocity, laser power and focusing, hatch spacing, and layer
thickness) must be optimized. It is worth noting that the thermo-
mechanical features of NiTiHf add to the complexity of fabrication. In
this paper, a Ti-rich NiTiHf alloy was processed for the first time via se-
lective laser melting (SLM), the most common AM technique for pow-
der metals. In addition, the mechanical and thermomechanical
features of SLM NiTiHf compared to conventionally processed alloy
were investigated.
A slightly Ti-rich Ni49.8Ti30.2Hf20 (at.% of measured composition)
alloy was produced by vacuum induction skull melting process. Part of
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
Table 1
ICP values obtained for as-extruded, powder, and SLM NiTiHf components.
Sample Weight (wt%) Ni (at.%) Ti (at.%)
As-extruded 171.2 Ref. Ref.
Powder 150.9 −0.03 0.06
SLM 84.3 −0.21 0.00
by hot extrusion at 900 °C (alloy designated as-extruded). Hot extrusion
was aimed to improve the transformation strain levels, cyclic stability,
and two-way shape memory effect (TWSME) of as-cast NiTiHf alloy
[2]. Other ingots were subjected to an Electrode induction-melting gas
atomization (EIGA) by TLS Technik GmbH (Bitterfield, Germany) to pro-
duce the powder. EIGA is a unique technique that produces spherical
powders with extremely low impurity (e.g., oxygen, carbon, ceramic
impurities, nitrogen) contents. A range of 25–75 μm particle fractions
was used to ensure a good compromise of layer resolution and
flowability. A SLM machine (Phenix Systems PXM) was used to produce
NiTiHf components directly from powder. The Phenix Systems PXM is a
powder-bed based SLM machine equipped with a 300 W Ytterbium
fiber laser manufactured by JK Lasers. The laser beam was directly fo-
cused via galvanometric mirrors producing a beam diameter of approx-
imately 80 μm, a beam quality of M2 b 1.2, and a collimated (TEM00)
beam with a Gaussian profile [35,36]. Prior to the fabrication, a CAD soft-
ware and a Phenix Systems software were used to create the 3D model
and to slice it into the requisite layers, respectively. In PXM machine, a
feeding piston moves upward to provide the powder. Subsequently, a
metal scraper and a metal roller collect, deposit, and compact the pow-
der layer on the building platform. Then, a laser selectively melts and
binds the powder particles to each other. Finally, the building piston
drops down with a layer thickness to accommodate the next layer.
This procedure is repeated until the fabrication of the fully dense com-
ponent is completed [33,37,38]. The fabrication procedure was conduct-
ed under argon atmosphere which decreased the oxygen level to
500 ppm. The SLM processing Parameters used in fabricating NiTiHf
components were considered to be 250 W laser power, 30 μm layer
thickness, 1.25 m/s scanning velocity, and 120 μm hatch spacing.
Chemical compositions of the as-extruded, powder, and SLM NiTiHf
were quantitatively evaluated using inductively coupled plasma atomic
emission spectroscopy (ICP-AES) for metallic elements and the LECO®
determinators for oxygen, nitrogen sand carbon content. To determine
Fig. 1. (a) SEM image of Powder, (b) particle distribution, (c) optical and (d) SEM images of SLM NiTiHf.
91
Hf (at.%) C (wt%) N (wt%) O (wt%)
Ref. 0.0040 0.0020 0.0433
−0.03 0.0053, 0.0054 0.0018, 0.0021 0.0623, 0.0626
0.22 – 0.0014 0.075
the basic microstructure of the alloys, the samples were mounted,
polished, etched, and imaged in a JEOL 840 SEM. Differential scanning
calorimetry (DSC) analyses were conducted using a TA Instruments
Q1000 with heating/cooling rate of 10 °C/min. Each specimen was cy-
cled 10 times between 0 and 370 °C to evaluate the stability of the
phase transformation temperatures. Martensite start (Ms) and martens-
ite finish (Mf) temperatures on cooling and austenite start (As) and aus-
tenite finish (Af) temperatures on heating were determined by tangent
technique. Thermomechanical tests of both as-extruded and SLM fabri-
cated samples were conducted using an MTS® 810 servo-hydraulic load
frame equipped with an Ameritherm NovaStar 7 kW induction heating
system. A Eurotherm controller was used to control the test tempera-
ture with type-K thermocouples, spot-welded directly to the middle of
the sample gage length. A heating rate of 20 °C/min was used while
cooling was partially controlled. Strains were measured from the dis-
placement of the platen surfaces using a Micro-Epsilon™ optoControl
2600, non-contacting LED based micrometer. Constant-force thermal
cycling was performed in compression at stresses ranging from 0 to
500 MPa. One SLM rectangular cube component with dimensions of
2 mm × 2 mm × 5 mm, fabricated in the horizontal direction was tested
under a minimum stress of 30 MPa due to the small sample size. The ex-
truded rods with a diameter of 5 mm and 10 mm long were tested
starting at 0 MPa. Then, each sample was cycled between 50 °C and
450 °C at a rate of 20 °C/min in 100 MPa increments from the lowest
stress to 500 MPa. Finally, each sample was tested at “0 MPa” to inves-
tigate their two-way shape memory.
Table 1 shows the ICP results comparing the compositions of pow-
der, as-extruded, and SLM NiTiHf. When compared to as-extruded ma-
terial, the level of Ni-loss are reported to be 0.03 at.% and 0.21 at.% for
the powder and SLM material, respectively. It can be inferred that the
SLM process more influence the Ni content rather than the powder
preparation procedure. Ni loss associated with SLM mostly can be at-
tributed to the fact that Ni element tend to evaporate sooner than the
92 M. Elahinia et al. / Scripta Materialia 145 (2018) 90–94
Fig. 2. DSC curves for Ni49.8Ti30.2Hf20 for SLM, powder, and as-extruded NiTiHf.
other two elements during the high power laser melting procedure [33].
The carbon, nitrogen, and oxygen level were also measured. In general,
the presence of oxygen and carbon contamination has been proven to
stabilize precipitates such as Ti4Ni2Ox-phase (referred to Ti2Ni-type),
TiO, and TiC within the NiTi matrix [39–41]. According to ICP results,
there is a small oxygen pick up in the powder and, as commonly seen
in most SLM NiTi alloys, there is additional oxygen content introduced
during the SLM process [42]. On the other hand, carbon pickup is almost
negligible during SLM process when compared to as-extruded alloy.
Therefore, it is expected to observe Ti4Ni2Ox-phase as well as TiO, but
not TiC, precipitates in SLM NiTiHf alloy.
The scanning electron microscopy (SEM) image of the powder is
shown in Fig. 1a and the particle size distribution is shown in Fig. 1b.
The average size of the particles were determined as 35 μm. Fig. 1c
and d show the optical microscopy and the SEM images of the SLM
NiTiHf, respectively. The optical image of SLM NiTiHf clearly displays
the formed micro-cracks and melts pools during fabrication. The
micro-crack formation can be attributed to thermal stresses resulting
from rapid solidification [33]. The SEM image of SLM NiTiHf illustrates
that tiny pores and finely dispersed nano-sized particles are presented
in the SLM NiTiHf. It is expected that these pores and the associated par-
ticles (e.g., oxides and carbides) can be tuned or reduced by optimizing
the laser parameters.
Fig. 2 demonstrates the DSC curves of as-extruded, powder, and SLM
NiTiHf. For the SLM part, the Ms, Mf, As, and Af were found to be 257, 193,
273, and 331.5 °C, respectively. The DSC results show that Ms decreases
after powder atomization and increases slightly after SLM. The increase
in TTs is mostly attributed to the preferential evaporation of nickel dur-
ing SLM processing which shifts the matrix composition to higher
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.
titanium content that typically leads to an increase in the TTs [33,43].
The ICP results in Table 1 also confirm the Ni evaporation after SLM pro-
cessing. When compared to the as-extruded material, the TTs of the SLM
material are slight lower, although it is expected to see higher TTs for
SLM due to the less Ni in the matrix. This observation can be explained
via ICP results, where higher level of oxygen content was observed for
SLM NiTiHf alloy. In general, the solubility of oxygen is almost negligible
in the NiTi matrix, and therefore, the extra oxygen results in the possible
formation of Ti4Ni2Ox-phase as well as TiO precipitates, which in turn
deplete Ti (or increase Ni) in the NiTi matrix [44,45]. Finally, the overall
increase in Ni/Ti ratio within NiTiHf matrix increase the TTs, as have
been proved by Tang et al., [46] Khalil-Allafi et al., [47]or Frenzel et al.,
[48]. Another observation here is that the SLM material demonstrates
broader transformation range compared to as-extruded, mostly attrib-
uted to the inclusions during SLM procedure as shown in Fig. 1d [49].
It should be noted that the samples are not homogenized after SLM
fabrication.
Fig. 2 also evaluates the thermal stability which is essential for most
NiTiHf applications [18]. All three alloys exhibit good thermal stability,
showing a degradation of TTs for the first cycle, after which the TTs re-
mains approximately constant. The high TTs drop after the first cycle
is mostly attributed to the so-called “stabilization effect”, which is
vanished after the first cycle.
Fig. 3 demonstrates the constant-force thermal cycling response of
Ni49.8Ti30.2Hf20 under applied constant compressive stress levels, and
the corresponding stress-free thermal cycling responses tested after
the experiments for as-extruded and SLM components to evaluate the
TWSME. From a grander perspective, both the as-extruded and SLM
NiTiHf demonstrate very similar thermomechanical responses under
the imposed stress. It is shown the SLM material exhibited larger hyster-
esis in agreement with the DSC data of Fig. 2. It is expected that this be-
havior ensues from the as-extruded parts and can be improved after
solution heat treatment as shown in other NiTi-based systems [50].
Moreover, comparing the stress-free response before and after the ex-
periments, the shape memory response is improved for both as-extrud-
ed and SLM sample indicative of two-way shape memory response,
although exhibiting small magnitudes (labeled “post” in Fig. 3). It is
worth noting that in cases where the two-way shape memory proper-
ties are desirable, appropriate training procedures are required.
Fig. 4a demonstrates a summary of the transformation temperatures
obtained in each cycle under different selected stress levels up to
500 MPa for both as-extruded and SLM NiTiHf alloys. Almost in all
cases the TTs attributed to as-extruded is higher than SLM alloy.
Again, this observation can be explained by the fact that SLM alloy con-
tains higher level of oxygen, and therefore, higher amount of TiO and/or
Ti4Ni2Ox-phases leading to lower TTs [26,48]. In general, TTs increase
with applied stress. Further, thermal hysteresis, measured as AF–MS,
 M. Elahinia et al. / Scripta Materialia 145 (2018) 90–94
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
for SLM material with increasing stress from 0 to 500 MPa. Fig. 4b dem-
onstrates transformation strain at each cycle for both as-extruded and
SLM NiTiHf alloys. At elevated levels of stress (100–500 MPa), a greater
net shape change is observed for SLM material compared to as-extrud-
ed. The transformation strain increased from 0.24% to 1.26% for the as-
extruded and from 0.24% to 1.52% for SLM when the applied stress
was increased from 100 to 500 MPa, respectively. Higher stress levels
are able to reorient more of the martensite twins in an orientation
that favor the applied strain during reverse transformation, which result
in the availability of more strain to be recovered during the forward
transformation. In general, there exists a critical point for each alloy
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
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-
strates that the irrecoverable strain increase with higher level of applied
stress for both cases. It can be observed that the irrecoverable strains of
two materials are essentially identical.
In summary, in this paper, using a selective laser melting system by
Phenix/3D Systems of type PXM, NiTiHf rectangular cubes were directly
manufactured using powder material. Subsequently, the thermal and
functional properties of SLM NiTiHf components were evaluated via
DSC and thermomechanical testing and are compared to as-extruded
NiTiHf. Composition analysis shows Nickel loss and oxygen pick up
after SLM processing due to the associated high power laser melting.
Finely dispersed particles, pores and cracks were observed after SLM.
Thermal analysis demonstrates that the TTs are slightly shifted to
lower values after SLM processing compared to the as-extruded
93
material. This is likely attributed to the formation of secondary Ti-rich
phases during atomization and SLM technique. The microstructural
analysis confirms the existence of Ti-rich secondary phases. The con-
stant-force thermal cycling response of SLM material demonstrated
higher transformation strains, but identical trend, with as-extruded ma-
terial. Finally, the stress-free thermal cycling responses of both SLM and
as-extruded material exhibited small magnitudes of two-way shape
memory. The microstructure and laser optimization will be a subject
of our future activity. Further, before transition into more complex
shapes, this material will be further evaluated and examined in tension
and/or torsion to find out the effect of inclusions and cracks on the func-
tional response and durability.
Acknowledgements
Funding support from the NASA Glenn Research Center, Transforma-
tional Tools & Technologies (TTT) Project is gratefully acknowledged
(contract #NNC16VA75P).
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