Materials and Design 111 (2016) 592–599

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Materials and Design

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Evaluation of mechanical and wear properties of Ti\\xNb\\7Fe alloys

designed for biomedical applications
S. Ehtemam-Haghighi a,⁎, K.G. Prashanth b, H. Attar a, A.K. Chaubey c, G.H. Cao d, L.C. Zhang a,⁎
a
School of Engineering, Edith Cowan University, 270 Joondalup Drive, Joondalup, Perth, WA 6027, Australia
b
Erich Schmid Institute of Materials Science, Austrian Academy of Sciences, Jahnstraße 12, A-8700 Leoben, Austria
c
Institute of Minerals and Materials Technology (IMMT), Bhubaneshwar, 751013, India
d
Department of Materials Engineering, Shanghai Key Laboratory of Modern Metallurgy and Materials Processing, Shanghai University, 149 Yanchang Road, Shanghai 200072, China

H I G H L I G H T S G R A P H I C A L A B S T R A C T

• Nb addition reduces the α" martensitic

phase content in the alloys microstruc-
ture.
• Nb content is inversely proportional to
the elastic modulus, hardness and com-
pressive strength of the alloys.
• The close relationship between the
wear resistance, microstructures and
mechanical properties of the alloys is
discussed.
• β-type Ti-11Nb-7Fe exhibits better
combination of properties than CP-Ti
and Ti-6Al-4V for orthopaedic applica-
tion.

a r t i c l e i n f o a b s t r a c t

Article history: A group of Ti\\xNb\\7Fe (x = 0, 1, 4, 6, 9, 11 wt.%) alloys was designed and produced by cold crucible levitation
Received 27 April 2016 melting process. The microstructural characteristic of the alloys with Nb addition and its effect on their mechan-
Received in revised form 6 September 2016 ical properties as well as wear resistance were investigated. Microscopic and phase analysis results show that all
Accepted 8 September 2016
the alloys, except for the Ti\\11Nb\\7Fe, exhibit orthorhombic α“ and body-centred cubic β phases, while
Available online 13 September 2016
Ti\\11Nb\\7Fe alloy consists of only β phase. It is proposed that increasing the Nb content enhances β phase sta-
Keywords:
bility and its proportion in the microstructure of the designed alloys. Depending on the proportion of β and α”
Titanium alloy phases, Ti\\xNb\\7Fe alloys show varied hardness (3.57–5.92 GPa) and compressive strength (1990–
Microstructure 2093 MPa). Additionally, they present wear rates in the range of 3 × 10−15–1 × 10−13 m3/m which correlates
Mechanical property well with the changes in the corresponding microstructures and mechanical properties. Among the studied al-
Wear loys, Ti\\11Nb\\7Fe with β phase microstructure, presents the lowest elastic modulus (86 GPa) and the highest
compressive strain (41.5%) along with high compressive strength, hardness and wear resistance. Therefore, it is
suggested that this β-type Ti\\11Nb\\7Fe alloy is a promising candidate, more suitable than the commercially
used CP\\Ti and Ti\\6Al\\4V, for orthopedic applications.
© 2016 Elsevier Ltd. All rights reserved.

1. Introduction
⁎ Corresponding authors.
E-mail addresses: sehtemam@our.ecu.edu.au, sehtemam@gmail.com An increasing aging population along with expectations of a high
(S. Ehtemam-Haghighi), l.zhang@ecu.edu.au, lczhangimr@gmail.com (L.C. Zhang). quality of life has led to a growing demand for the development of

http://dx.doi.org/10.1016/j.matdes.2016.09.029
0264-1275/© 2016 Elsevier Ltd. All rights reserved.
 S. Ehtemam-Haghighi et al. / Materials and Design 111 (2016) 592–599
novel metallic biomaterials for replacing dysfunctional load-bearing
bone tissues [1]. Among metallic biomaterials, titanium (Ti) and its
alloys have been widely used for orthopedic applications due to
their remarkable combination of good mechanical properties, high
biocompatibility and excellent corrosion resistance [2–6]. However,
despite their attractive performance there are still challenges facing
their application in artificial joints [7]. These concerns are mainly re-
lated to bio-toxicity, the need for lower elastic modulus and better
wear resistance. For instance, both Al and V elements in Ti\\6Al\\4V,
the most widely applied Ti alloy, are considered to induce long-term
health problems such as haematological alterations and Alzheimer's
diseases [8,9]. Additionally, although the elastic modulus of Ti alloys
is lower than other common metallic biomaterials (e.g. 316 L stain-
less steel and Co\\Cr alloys), it is still higher than that of human
bone [10,11]. The significant difference between the elastic modulus
of the implant material and the surrounding bone may induce stress
shielding effect, whereby the bone is prevented from supporting
loads useful to its health [12–14]. This may result in bone resorption
around the implant and eventual loosening of the implant [15–17].
Poor tribological properties have also been considered as a reason
for the failure of an implant due to the release and accumulation of
metal wear debris in surrounding tissues, thereby causing adverse
allergic tissue reactions and a reduction in the service life of the im-
plant [10]. Wear of dentures and wear of screws and plates used in
bone fracture repair are good examples of biomedical applications
where good tribological properties are needed [18]. Therefore,
good wear properties play a key role in controlling and determining
the long-term service of Ti alloys.
To improve the wear resistance of Ti alloys a variety of methods have
been explored, such as thin film surface modification [19], titanium ma-
trix composites [20] and additive manufacturing technology for fabri-
cating Ti based materials [21]. However, weak adhesion of thin film to
substrate, undesirable increase in elastic modulus and poor surface
quality, respectively, have been the major constraints identified in
using these methods [19,22,23].
Therefore, the design of new Ti alloys composed of non-toxic ele-
ments showing not only high strength and hardness but also lower elas-
tic modulus and improved wear resistance when compared to the
conventional Ti alloys is desirable. It has been suggested that β-type Ti
alloys possess lower elastic modulus, higher strength and hardness as
well as excellent abrasive and wear resistance than α and α + β-type
Ti alloys [24–26]. Consequently, during the last decade, extensive re-
search has focused on designing new β-type Ti alloys containing non-
toxic elements such as Mo, Nb, Fe, Sn, Zr and Ta targeting the optimiza-
tion of mechanical properties [27,28]. Examples of these alloys include
Ti\\Mo [29], Ti\\29Nb\\13Ta\\4.6Zr [30], Ti\\24Nb\\4Zr\\7.9Sn [31]
and Ti\\10Zr\\15Nb\\15Si [32].
It has been reported that Fe is a non-toxic, low cost and biocompat-
ible β-stabilizer element for developing Ti alloys with high strength
[33–35], while biocompatible, β-stabilizer Nb contributes to a decrease
in the elastic modulus of the alloy, also required for orthopedic applica-
tion [36,37]. Hsu et al. [38] investigated the microstructure, bending
modulus, bending strength as well as biocompatibility of the as-cast
Ti\\5Nb\\xFe alloys up to 5 wt.% Fe addition. Based on their study,
Ti\\5Nb\\2Fe exhibits the lowest bending modulus which is lower
than that of CP\\Ti by 20%. Additionally, it shows the highest bending
strength to modulus ratio which is larger than that of CP\\Ti by 214%.
Moreover, preliminary cell culturing results suggested that the
Ti\\5Nb\\xFe alloys are biocompatible and support cell attachment
[38]. Chaves et al. [39] studied the influence of phase transformation
on the elastic modulus of Ti\\xNb\\3Fe alloy system with Nb content
ranging from 10 to 25 wt.%. According to their study, increasing the
Nb content improves the β phase stability and reduces the elastic mod-
ulus of the alloys [39]. Ushida et al. [40] studied the mechanical proper-
ties and biocompatibility of Ti\\Fe\\Nb\\Zr alloy system with Fe
addition through thermo-mechanical treatments. According to their
593
work, the hardness of the alloys decreases with Fe addition up to
7 mol% and subsequently increases by further Fe addition due to solid
solution strengthening. Their results showed that among the alloys, so-
lution treated Ti\\5Fe\\3Nb\\3Zr possesses the lowest elastic modulus.
Additionally, it shows higher tensile strength and better biocompatibil-
ity than the annealed Ti\\6Al\\4V ELI alloy [40].
Since there is relatively limited literature on the properties of Ti\\Fe
based alloys with Nb addition, this study intends to investigate the ef-
fect of Nb on the microstructure of the designed Ti\\xNb\\7Fe alloys.
It also investigates its influence on the mechanical properties including
hardness, elastic modulus, compressive yield strength, compressive
strength and strain as well as wear responses of the alloys in order to as-
sess their suitability for orthopedic application. This study indicates that
the alloy design plays a key role in tailoring the mechanical and wear
properties of Ti alloys required for biomedical application.
2. Experimental
A series of Ti\\xNb\\7Fe (x = 0, 1, 4, 6, 9, 11 wt.%) alloys was de-
signed and fabricated from 99.9 wt.% pure Ti, Fe and Nb using a cold cru-
cible levitation melting method (CCLM) under the protection of an
argon atmosphere in a water-cooled copper crucible. The CCLM furnace,
a type of induction melting furnace, was comprised of induction coils
which were wrapped around a water cooled copper crucible and con-
nected to a frequency inverter power supply. After the raw metals
were completely melted and mixed adequately, the electric power
was cut off and the molten metals were quenched in the water-cooled
copper crucible. The alloy ingots were flipped and re-melted four
times to obtain homogeneity in their chemical composition. The dimen-
sions of as-cast alloys were 8 mm in diameter and 100 mm in length.
The as-cast samples were sectioned perpendicular to their longitudinal
direction using a Buehler Isomet low speed diamond saw to obtain
specimens. Prior to microstructural study, the samples were ground
and polished using standard metallographic procedures, followed by
etching in Kroll's solution (5 vol% HF, 30 vol% HNO3 and 65 vol% H2O).
These studies were then conducted using a scanning electron microsco-
py (SEM, JEOL JSM 6000). Constituent phases of the alloys were deter-
mined by X-ray diffraction (XRD) using a PANalytical EMPYREAN
diffractometer with Co Kα radiation (λ = 0.1789 nm) operated at
40 kV and 40 mA. The integrated areas for α″ and β diffraction peaks
in the XRD patterns were calculated by using the peak-fitting program,
Fityk, with Pearson VII function [41–43]. Based on the integrated areas,
the volume fraction (Vf) of each phase was estimated in a similar man-
ner to Ref [44] using the following equations:
Aαʺ
V f ðαʺ Þ ¼ ð1Þ
Aαʺ þ Aβ
Aβ
V f ðβ Þ ¼ ð2Þ
Aαʺ þ Aβ
where Vf(α″) and Vf(β) are the volume fractions and Aα″ and Aβ are the
total integrated areas, corresponding to α″ and β phases, respectively.
Evaluation of the mechanical properties of the alloys was based on
nanoindentation and compressive tests. The hardness and elastic mod-
ulus of the samples were measured by a nanoindentation test using a
UMIS equipment from Frischer-Cripps laboratories with a Berkovich in-
denter applying a maximum load of 400 mN. At least 25 indentations
were carried out on the metallographically polished surface of each
sample and the average values of the hardness and elastic modulus
were attained. To determine the compressive yield strength, compres-
sive strength and strain of the alloys, a compressive test was carried
out on the cylindrical samples with a diameter of 8 mm and a height
of 16 mm using an Instron 5980 universal testing machine at a cross-
head speed of 0.001 mm/s.
594 S. Ehtemam-Haghighi et al. / Materials and Design 111 (2016) 592–599
Sliding wear tests were performed according to the ASTM G 99-05
standard at room temperature and in ambient atmospheric conditions
using a pin-on-disc device. A hard-faced stainless steel disc of 45 mm
in diameter and 13 mm in thickness was applied against the as-cast al-
loys (flat pins of 8 mm in diameter and 25 mm in height). The wear tests
were performed at a fixed load of 25 N with a sliding speed of 0.5 m/s for
15 min. The rate of wear was measured using the following equation
[21]:
Vs
Qs ¼
Ls
where Qs is the wear rate, Vs is the sliding volume loss and Ls is the
sliding distance. The volume loss was measured from the wear loss de-
termined by calculating the weight of the flat head pins before and after
tests. The sliding distance is given by Ls = 2π rs vs ts where rs is the radius
of the wear track (22.5 mm), vs is the speed in rounds per minutes (240
rpm) and ts is the time (15 min). Thereafter, the worn surface of the
samples was evaluated using SEM.
3. Results and discussions
Fig. 1 presents the XRD profiles of a series of Ti\\xNb\\7Fe alloys.
Ti\\7Fe is comprised of the body-centered cubic (bcc) β phase with
the least volume fraction (Vf, β = 62%) and the highest concentration
of the orthorhombic α″ martensitic phase (Vf, α″ = 38%). This fast
cooling induced α″ orthorhombic structure is obtained from a distorted
hexagonal unit cell in which the c-axis of the orthorhombic unit cell cor-
responds to the c-axis of the hexagonal unit cell, whereas a and b corre-
late with the orthogonal axis of the hexagonal unit cell [4].
When 1 wt.% Nb is added, the resultant alloy shows the same crystal-
line structure as that of Ti\\7Fe. However, the intensity of β phase peaks
increases, suggesting an increase in the volume fraction of the β phase
(Vf, β = 66%) and reduction of that of the α″ phase (Vf, αʺ = 34%).
With addition of 4 or 6 wt.% Nb to Ti\\7Fe, the intensity of β peaks,
hence the proportion of the β phase increases (Vf, β = 82% and 90% re-
spectively), while the number of the α″ phase peaks, and correspond-
ingly α″ phase concentration, decrease further. When Nb content is
9 wt.%, the alloy shows a very weak peak of the α″ phase in the XRD pat-
tern suggesting that an increased amount of the β phase is retained in
the alloy microstructure (Vf, β = 96%). Finally, with addition of
11 wt.% Nb, the peaks corresponding to the α″ phase completely disap-
pear, while only peaks from the β phase are observed, indicating the
Fig. 1. XRD profiles of as-cast Ti\
\xNb\
\7Fe alloys.
alloys microstructure contains only the β phase. In order to study
whether ω phase is present in the studied alloys or not, XRD at lower
scanning speed was also carried out. Generally, the presence of ω
phase could be detected by conducting XRD at lower scanning speed
(0.5°/min) [1,45]. In the present study, the XRD patterns at lower scan-
ning speed (not shown here) did not contain the peaks related to ω
phase suggesting the absence of this phase in the Ti\\xNb\\7Fe alloys
microstructure.
The SEM microstructures of the as-cast Ti\\7Fe and ternary
Ti\\xNb\\7Fe alloys are shown in Fig. 2. Coexistence of the α″ martens-
ð3Þ
ite and β phase is evident in all alloys except for Ti\\11Nb\\7Fe in
which only the β phase is observed. As shown in Fig. 2(a), Ti\\7Fe ex-
hibits the highest concentration of the α″ martensitic phase in the β ma-
trix. With the addition of Nb up to 9 wt.%, the proportion of the α″ phase
decreases (Fig. 2(b–e)). With a further increase in Nb content to 11 wt.%,
the stability of the β phase is effectively enhanced so that the micro-
structure of the alloy consists entirely of β phase (Fig. 2(f)). It should
be noted that the microstructural observations are in good agreement
with the corresponding XRD patterns. The average β grain size of the
Ti\\xNb\\7Fe alloys was estimated to be in the range of 144–175 μm.
The average β grain size of the alloys decreases with increasing the Nb
contents, possibly due to Nb-grain boundary interaction which slows
the grain boundary growing [46].
Based on the above results it can be deduced that the addition of
more Nb to Ti\\7Fe alloy promotes the stabilization of the β phase
and decreases the possibility of β to α″ martensitic transformation in
the alloys during rapid cooling. To be more precise, by increasing the
Nb content of the alloys, the β to α″ martensitic transformation temper-
ature, Ms, decreases, hence the concentration of the α″ phase in the
quenched alloys declines.
Table 1 presents the hardness and elastic modulus values of the
studied alloys measured by nanoindentation test. It can be inferred
from Table 1 that the aforementioned properties of the alloys are sensi-
tive to their β-stabilizer Nb content. The highest values for hardness
(5.92 GPa) and elastic modulus (130 GPa) are observed in Ti\\7Fe
alloy which has the highest proportion of α″ martensite in its micro-
structure (Vf, α″ = 38%). By increasing the Nb content of the alloys up
to 11 wt.%, hence decreasing the volume fraction of the α″ phase, both
hardness and elastic modulus of the alloys decline, reaching the mini-
mum values of 3.57 GPa and 86 GPa, respectively, in the Ti\\11Nb\\7Fe
alloy with an exclusively β phase microstructure. Consequently, the
progressive reduction in the measured hardness and elastic modulus
values of the Ti\\xNb\\7Fe alloys with Nb addition can be ascribed to
the decrease in their α″ phase concentration. In fact, there are different
reports on elastic modulus and hardness of α″ and β phases in Ti alloys.
While Lee et al. [47] found that in their binary Ti\\Nb system the β and
α” phases exhibit similar values of hardness and elastic modulus,
Matlakhova et al. [48] and Zhu et al. [49] reported higher elastic modu-
lus and hardness for α″ than β phase which is consistent with the pres-
ent study. The hardness of all alloys examined in this study are larger
than that of the commercially used biomedical CP\\Ti (2.7 GPa) [32].
In addition, the hardness values for Ti\\xNb\\7Fe (x = 0, 1, 4 wt.%)
are greater than that of Ti\\6Al\\4V (4.2 GPa) [50]. Moreover, among
the studied alloys, Ti\\xNb\\7Fe (x = 6, 9, 11 wt.%) alloys, with higher
proportions of the β phase, present lower elastic modulus values than
those of CP\\Ti (112 GPa) [32] and Ti\\6Al\\4V (125 GPa) [50].
Table 1 also summarizes the compressive strength, 0.2% proof com-
pressive yield strength, and compressive strain of the Ti\\xNb\\7Fe al-
loys. Only Ti\\7Fe and Ti\\1Nb\\7Fe alloys failed during the test, while
other alloys deformed until the maximum load capacity (100 kN) of the
machine was reached and the test was stopped. According to Table 1,
Ti\\7Fe and Ti\\1Nb\\7Fe alloys, with the two highest α″ martensitic
phase concentrations, present the two lowest fracture strains (7.9%
and 10.0% respectively).
As the Nb content rises to 4 wt.%, the formation of the α″ phase dur-
ing quenching decreases, leading to a subsequent increase in the
 S. Ehtemam-Haghighi et al. / Materials and Design 111 (2016) 592–599 595

Fig. 2. SEM microstructures of the etched Ti\

\xNb\
\7Fe alloys: (a) Ti\
\7Fe; (b) Ti\
\1Nb\
\7Fe; (c) Ti\
\4Nb\
\7Fe; (d) Ti\
\6Nb\
\7Fe; (e) Ti\
\9Nb\
\7Fe and (f) Ti\
\11Nb\
\7Fe.

maximum strain that the alloy endures. It is noted that further addition
of Nb (6, 9 and 11 wt.%) results in enhancement of the compressive
strain, reaching the highest value (41.5%) in Ti\\11Nb\\7Fe. Such in-
creases in the compressive strain with Nb addition can be attributed
to the reduction in hardness of the alloys [51], which is caused by the
decrease in the proportion of the α″ phase present in their microstruc-
ture (Fig. 2). The high compressive strain indicates good workability of
the alloy at room temperature [52]. According to Table 1, except for
Ti\\7Fe and Ti\\1Nb\\7Fe, the compressive strength of the alloys de-
creases with increasing Nb content. Since the orthorhombic crystal
structure of the α″ phase contains less slip systems than the bcc crystal
structure of β phase, higher stress is required for plastic deformation of
the α″ phase than for the β phase matrix [52,53]. Consequently, the ob-
served reduction tendency in the compressive strength of the
Ti\\xNb\\7Fe (x = 4, 6, 9, 11 wt.%) alloys can be explained by taking
into account the decrease in the volume fraction of a high strength α″
phase presents in the alloys microstructure as the Nb concentration in-
creases. In the case of Ti\\7Fe and Ti\\1Nb\\7Fe alloys, despite the
presence of large concentrations of a high strength α″ phase (Fig. 2(a),
(b)), their compressive strength is lower than that of other
Ti\\xNb\\7Fe alloys. This is because these two alloys are unable to en-
dure more plastic deformation at high stresses due to the low the ductile
nature of the α″ phase, hence they fail in the early stages of plastic de-
formation. While other alloys, which contain lower concentrations of a
low ductile α″ phase, do not fail during the test and present more plastic
deformation. Therefore, their compressive strength and strain increase
compared to Ti\\7Fe and Ti\\1Nb\\7Fe alloys. It is noteworthy noting
that the compressive strengths observed in the studied alloys are great-
er than those of typical biomedical Ti materials including CP\\Ti
(820 MPa) [54], Ti\\6Al\\4V (1300 MPa) [55] and even Ti\\TiB com-
posite materials (1420–1434 MPa) [23] produced by conventional and
advanced manufacturing technologies.

Table 1
Hardness (H), elastic modulus (E), compressive strength (σmax), compressive yield strength (σy), and compressive strain (εmax) values obtained in Ti\
\xNb\
\7Fe alloys.

Alloy nominal composition (wt.%) H (GPa) E (GPa) σmax(MPa) σy(MPa) εmax(%)

Ti\
\7Fe 5.92 ± 0.06 130 ± 1 1990 ± 8 1847 ± 5 7.9 ± 0.2
Ti\
\1Nb\\7Fe 5.58 ± 0.09 124 ± 2 1972 ± 12 1785 ± 7 10.0 ± 0.9
Ti\
\4Nb\\7Fe 5.13 ± 0.04 115 ± 2 2093 ± 17 1539 ± 11 24.3 ± 0.3
Ti\
\6Nb\\7Fe 4.18 ± 0.09 97 ± 3 2014 ± 14 1144 ± 7 32.1 ± 1.7
Ti\
\9Nb\\7Fe 3.72 ± 0.04 89 ± 1 2007 ± 15 1010 ± 9 40.5 ± 1.9
Ti\
\11Nb\\7Fe 3.57 ± 0.03 86 ± 1 2006 ± 14 985 ± 8 41.5 ± 1.6
596 S. Ehtemam-Haghighi et al. / Materials and Design 111 (2016) 592–599
Fig. 3. H/E ratio and wear rate of the Ti\
\xNb\
\7Fe alloys.
As can be inferred from Table 1, the compressive yield strengths of
the Ti\\xNb\\7Fe alloys are affected by Nb concentration. Among the
studied alloys, Ti\\7Fe with the highest concentration of α″ phase pre-
sents the highest compressive yield strength. Conversely, the yield
strength of the alloys reduces with increasing Nb concentration and
reaches a minimum in Ti\\11Nb\\7Fe alloy with an exclusively β
Fig. 4. SEM micrographs showing the wear morphology of worn surfaces of Ti\
\xNb\
\7Fe alloys: (a) Ti\
Ti\
\11Nb\ \7Fe.
phase microstructure. The decreasing trend observed in the compres-
sive yield strength of the alloys can be attributed to reduction in the pro-
portion of the α″ phase which contains fewer slip systems than the β
phase, hence requires higher stresses for deformation as explained
above. It should be noted that the compressive yield strength of all stud-
ied Ti\\xNb\\7Fe alloys are higher than those of the commonly used
biomaterials, CP\\Ti (552 MPa) [4] and Ti\\6Al\\4V (970 MPa) [56].
The high yield strength enhances the capacity of the alloy against its
permanent shape change which could benefit patients [52].
Therefore, it can be concluded that all the Ti\\xNb\\7Fe alloys pres-
ent much higher compressive strengths and compressive yield
strengths, which potentially make them suitable materials for bearing
heavy loading in implant applications [2,8].
Classical theories of wear show that hardness is a key parameter in
controlling the wear of a material, and a hard material usually possess a
high wear resistance [57]. In fact, it is increasingly realized that the wear
of a material is related to its ability to resist elastic strain to failure, which
is determined by the H/E (hardness to elastic modulus) ratio [57,58]. A
higher H/E ratio indicates better wear resistance of a material [32]. Fig. 3
presents the H/E ratio and wear rate variations of the alloys with respect
to their Nb concentration. As can be seen, with the addition of Nb, the H/
E of the alloys decreases. This trend indicates that the wear resistance of
Ti\\xNb\\7Fe alloys reduces with Nb addition, which concurs with an in-
crease in the alloys wear rate as demonstrated in Fig. 3. According to the
results shown in this figure, Ti\\7Fe alloy, with the highest α″ martensite
\7Fe; (b) Ti\
\1Nb-7Fe; (c) Ti\
\4Nb\
\7Fe; (d) Ti\
\6Nb\
\7Fe; (e) Ti\
\9Nb\
\7Fe and (f)
 S. Ehtemam-Haghighi et al. / Materials and Design 111 (2016) 592–599
concentration, possesses the largest H/E ratio (0.0455), hence the lowest
wear rate (3 × 10−15 m3/m). Upon addition of Nb, hence a decrease in
the proportion of the α” phase (Fig. 2), the wear rate increases from
1 × 10−14 m3/m for Ti\\1Nb\\7Fe to 1 × 10−13 m3/m for Ti\\11Nb\\7Fe
alloy with a single β phase microstructure.
As shown in Fig. 3, the Ti\\xNb\\7Fe alloys studied in this work pos-
sess a higher H/E ratio than the widely used Ti alloys, CP\\Ti (0.0241)
[32] and Ti\\6Al\\4V (0.0336) [50]. It is therefore expected the alloys
in this study will present better wear resistance. For instance, the
wear rate of cast CP\\Ti under similar conditions is observed to be
1.55 × 10−12 m3/m [21].
Fig. 4 presents the wear tracks of the cast alloys as a function of Nb
content. The wear tracks of the alloys show the presence of typical
wear features including wear scars, ploughing grooves, microcracks
and delamination. The Ti\\7Fe alloy shows shallow wear scars along
with the presence of some delamination cracks (Fig. 4(a)), which are
formed at the surface of the sample in contact with the counter disc
due to high strain levels developed during the wear test [21]. However,
since this alloy possesses a high hardness (Table 1), the cracks are un-
able to propagate into a complete delamination of surface which indi-
cates a high resistance of this alloy to wear. As seen in Fig. 4(b), with
the addition of 1 wt.% of Nb to the Ti\\7Fe alloy, the wear surface of
the alloy shows deeper wear scars and fewer signs of delamination
due to the lower hardness of this alloy compared to Ti\\7Fe.
Fig. 5. (a) XRD patterns and (b) EDX spectra of the Ti\
\7Fe and Ti\
\11Nb\
\7Fe alloys worn
surfaces.
597
Additionally, the presence of ploughing grooves is observed. With a fur-
ther increase in Nb content to 4 and 6 wt.%, the ploughing grooves get
deeper and delamination of the surface becomes more significant, pos-
sibly because of further reduction in the concentration of the α″ phase,
hence a decrease in the hardness of the alloys (Fig. 4(c–d)). Finally, with
the subsequent addition of 9 and 11 wt.% Nb complete delamination of
some parts of the surface is observed which indicates higher material
removal due to a further decrease in proportion of α″ phase, hence
hardness of the alloys (Fig. 4(e–f)). It should be noted that the micro-
structural observations of the samples after the wear test are consistent
with the wear rate trend shown in Fig. 3.
Fig. 5 presents the XRD patterns and EDX spectra of the worn surface
in Ti\\7Fe and Ti\\11Nb\\7Fe alloys. The XRD results indicate that the
worn surface of both alloys contain titanium oxide (TiO) (Fig. 5(a)). Ad-
ditionally, the XRD pattern of β-type Ti\\11Nb\\7Fe contains more TiO
peaks than that of (α″ + β) Ti\\7Fe alloy, which indicates that more TiO
is produced in the former alloy. The presence of a higher amount of ox-
ygen (9.31 wt.%) in Ti\\11Nb\\7Fe alloy than in Ti\\7Fe alloy
(2.24 wt.%) is also evident from the EDX spectra in Fig. 5(b).
It has been reported that during the wear test, sliding of a specimen
against a counter disc causes the release of friction heat and a subse-
quent increase in the contact temperature of the worn surface [59].
Due to the high reactivity of Ti, the high temperature can result in the
formation of oxides on the worn surface [60]. However, it has been
demonstrated that the oxides formed during wear are loosened and
brittle, hence do not provide protection from wear [59,61] and tend to
be continuously fragmented, producing wear debris [62,63]. Studies
have shown that according to Archard's wear equation [64], the wear
volume is inversely proportional to the hardness of the alloy under
investigation [64]. Therefore, in a lower hardness alloy, higher plas-
tic deformation of surface and sub-surface during wear causes
more delamination and production of a higher volume of metallic
wear debris which can be oxidized at high frictional temperatures
[59]. This leads to an increase in the roughness of the alloy surface
which results in a higher abrasion and wear rate [65] compared to
a higher hardness alloy, as can also be seen in Fig. 3. The existence
of more oxide particles in the lower hardness Ti\\11Nb\\7Fe alloy
is also evident in Fig. 4(f), in contrast with the higher hardness
Ti\\7Fe alloy shown in Fig. 4(a). As such, the higher oxygen content
in Ti\\11Nb\\7Fe alloy than in the Ti\\7Fe alloy (Fig. 5) can be ex-
plained by taking into account the lower hardness of the
Ti\\11Nb\\7Fe alloy which results in the presence of a higher pro-
portion of oxide debris on its worn surface.
The wear mechanisms observed in the Ti\\xNb\\7Fe samples are
similar to those of the widely used Ti alloys, CP\\Ti and Ti\\6Al\\4V,
where wear takes place as a result of abrasive and oxidative processes
[21,62]. The abrasive process is responsible for the ploughing grooves
and formation of cracks that propagate and lead to delamination of
the surface and material removal [21]. According to the results, although
the wear mechanisms operating in Ti\\xNb\\7Fe alloys, CP\\Ti and
Ti\\6Al\\4V are similar, the Ti\\xNb\\7Fe family of alloys are expected
to have a lower wear rate, or in other words, better wear resistance, be-
cause of the higher H/E ratio observed in the alloys which makes them
strong competitors for use in biomedical applications.
Based on these results, it can be concluded that addition of Nb con-
siderably affects the properties of the studied Ti\\xNb\\7Fe alloys.
Among these, Ti\\11Nb\\7Fe presents the best combination of me-
chanical properties, including the lowest elastic modulus (86 GPa) and
the highest compressive strain (41.5%). Additionally, it exhibits com-
pressive strength (2006 MPa) and compressive yield strength
(985 MPa) higher than those of CP\\Ti (820 MPa and 552 MPa) [4,54]
and Ti\\6Al\\4V (1300 MPa and 970 MPa) [55,56], as well as a hardness
(3.57 GPa) greater than that of CP\\Ti (2.7 GPa) [54]. Furthermore, de-
spite the higher wear rate of this alloy in comparison to the other stud-
ied Ti\\xNb\\7Fe alloys, it is expected that it will possess better wear
resistance compared to CP\\Ti and Ti\\6Al\\4V. The combination of
598 S. Ehtemam-Haghighi et al. / Materials and Design 111 (2016) 592–599
mechanical properties indicates that the Ti\\11Nb\\7Fe alloy has a
potential for use in orthopedic applications.
4. Conclusion
In this study, the effect of Nb on the microstructure of the designed
Ti\\xNb\\7Fe alloys, the resulting mechanical properties and the
wear response of the alloys was investigated. The main results are sum-
marized as follows:
1. The XRD analysis revealed that Ti\\7Fe alloy is comprised of β and α″
phases. As more Nb is added to this alloy (1, 4, 6, 9 wt.%), the concen-
tration of the α″ phase decreases, while the proportion of the β phase
increases reaching a maximum in Ti\\11Nb\\7Fe alloy with an ex-
clusively β phase microstructure.
2. The microstructural studies performed by XRD analysis and SEM
showed that increasing the Nb content enhances the stability of the
designed alloys against β to α″ martensitic transformation during
quenching.
3. The compressive strength (1990–2093 MPa), compressive yield
strength (985–1847 MPa) and hardness (3.57–5.92 GPa) of the
Ti\\xNb\\7Fe alloys are higher than those of the widely used CP\\Ti
(820 MPa, 552 MPa and 2.7 GPa,) or Ti\\6Al\\4V (1300 MPa,
970 MPa and 4.2 GPa) materials.
4. Among the studied alloys, Ti\\7Fe exhibits the highest elastic modu-
lus (130 GPa), while β-type Ti\\11Nb\\7Fe alloy shows the lowest
elastic modulus (86 GPa) which is smaller than those of CP\\Ti
(112 GPa) and Ti\\6Al\\4V (125 GPa).
5. The wear resistance of Ti\\xNb\\7Fe alloys reduces by increasing
their Nb content. However, it is expected that alloys will show better
wear resistance than the widely used CP-Ti and Ti\\6Al\\4V.
6. Among the alloys, Ti\\11Nb\\7Fe presents a favourable combination
of properties for orthopedic application.
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