CHARACTERIZATION AND COMPARISON OF MECHANICAL PROPERTIES

AND CORROSION RESISTANCE OF TI-10Mo-20Nb, TI-6Al-4V AND TI-Cp

ALLOYS FOR BIOMEDICAL APPLICATIONS

Patrick de Lima Vieira

UniFOA, Graduação em Engenharia Mecânica
Volta Redonda, Rio de Janeiro
http://lattes.cnpq.br/6827457061434519
Lucas de Mendonça Neuba
Instituto Militar de Engenharia, Pós-graduação em Ciência dos Materiais, SE/8
Rio de Janeiro, Rio de Janeiro
http://lattes.cnpq.br/8936653944979318
Raí Felipe Pereira Junio
Instituto Militar de Engenharia, Pós-graduação em Ciência dos Materiais, SE/8
Rio de Janeiro, Rio de Janeiro
http://lattes.cnpq.br/8990097179504095
Sergio Neves Monteiro
Instituto Militar de Engenharia, Pós-graduação em Ciência dos Materiais, SE/8
Rio de Janeiro, Rio de Janeiro
http://lattes.cnpq.br/2962183322412029
Abstract: Due to one of the main biomedical alloys, the Ti-6Al-4V alloy, over
time generate oxides of V and Al that accumulate in the body and cause
cytotoxic effects. Researches have been making an effort for developing β
metaestable Ti alloys that combine corrosion resistance, biocompatibility and
good mechanical properties. In view of this scenario, the present work aims to
characterize a Ti-10Mo-20Nb alloy and compare the results obtained with a Ti-
cp alloy and Ti-6Al-4V alloy. The Ti-10Mo-20Nb samples have been subjected
to heat treatment at 1000°C, after that they have been water quenched and a
hot swagging process at 900°C have been applied resulting on a cross section
reduction of 80%. The alloys have been characterized by optical microscopy,
scanning electron microscopy (SEM), Vickers microhardness and the linear
polarization technique. For the Ti-10Mo-20Nb alloy the ratio between the
hardness and the elastic modulus was of (3.22), the hardness value (238 HV)
and the elastic modulus (74 GPa). The Ti-10Mo-20Nb alloy showed a better
mechanical and biological compatibility due to the non-cytotoxic alloy elements,
Mo and NB, but the lower corrosion resistance value when compared to other
alloys, however it is still very resistant to corrosion and has a remarkable
passivation layer. Being a promising alternative for biomedical applications due
to the better biocompatibility with human bone.
Keywords: Ti-10Mo-20Nb; Linear polarization; SEM; Vickers microhardness;
biomaterial.
 1. INTRODUCTION

Titanium (Ti) and its alloys are widely used as materials for orthopedic
implants. This is due to its excellent mechanical property, satisfactory
biocompatibility, low density and low elastic modulus compared to stainless
steel alloys or based on Co-Cr alloys, both used as orthopedic biomaterials
(NOURI et al., 2015; CHEN et al., 2015; GEETHA et al., 2013). However, many
Ti alloys, such as Ti-6Al-4V, are at risk of releasing toxic ions such as aluminum
(Al) and Vanadium (V). The release of these ions causes a series of cytotoxic
effects over time and promotes the appearance of diseases such as
Alzheimer's and other mental disorders (KRÖGER et al., 1998).

Therefore, an urgent demand for the development of new Ti alloys that

have non-toxic elements such as Mo, Zr, Sn, Ta and Nb (FERRANDINI et al.,
2007; GUO et al., 2014; JUNG et al., 2013). The addition of beta (β) stabilizers
can reduce the elastic modulus, contributing to the increase of the implant
lifetime since avoids the stress shielding phenomenon. This occurs when the
implant is on a direct contact with the bone tissue and have a higher elastic
modulus than the bone, the difference will cause a resorption on the bone,
weakening the bone structure around the implant (JOSHI et al., 2000; SUL,
2003).

The titanium β alloys provides an excellent corrosion resistance for the

human body fluids, as well as display a low Young’s modulus and a better
hardness property when compared to the Ti α e Ti α + β alloys. Many authors
investigated different Ti-Mo-Nb alloys as possible orthopedic implants
candidates by their good mechanical properties and outstanding corrosion
resistance in conditions that simulate the body fluids (CHELARIU et al., 2014;
XU et al., 2008, 2013). Although Ti and Nb possess a relatively high elastic
modulus when compared to the bone tissue (LEVINE et al., 2006; MATSUNO et
al., 2001; RHO et al., 1993), the niobium (Nb) as an alloying element of the
titanium alloy provides the acquisition of alloys having lower elastic modulus
(NNAMCHI et al., 2016; ZHOU et al., 2008).
 Therefore, the present study seeks to investigate the microstructure,
corrosion potential and mechanical properties of the Ti-10Mo-20Nb alloy and
compare them with Ti commercially pure (cp) and Ti-6Al-4V alloys. The Ti-
10Mo-20Nb ingot received heat treatment at 1000 °C for 24 hours by means of
a tubular furnace and was then quenched in water at room temperature.
Thereafter, the ingot has been forged at 900 °C which reduced its area to a total
of 80% approximately. The Ti-10Mo-20Nb can be a possible replacement for
the Ti-6Al-4V alloy, currently one of the most employed, although releases
toxical ions causing injuries to the human health throughout life.

2. Materials and methods

Ti-cp, Mo-cp and Nb-cp an alloy was obtained by arc fusion process with
a tungsten electrode and an argon atmosphere, the obtained ingot received a
heat treatment at 1000 °C for 24 hours using a tubular furnace and then
quenched in water at room temperature. A forging process was carried out at
900 °C and generated an 80% reduction in the cross section. In addition, two
plates of Ti-6Al-4V (10 x 20 x 1 mm) and other two thin plates of Ti-cp (10 x 20
x 1 mm), have been used.

The linear polarization corrosion test was performed using the equipment
GALVANOSTAT AUTOLAB model PGSTAT302N. In a support container, the
sample was introduced in such a way as to leave only the area of the sample's
contact surface in contact with the fluid of the 0.9% NaCl ringer's solution in
distilled H2O, which will later fill the container. The tests were carried out in a
cell with three corrosion electrodes. A platinum wire and an Ag / AgCl electrode
saturated in KCl (calomel) solution were used as counter electrode and
reference electrode, respectively. The linear polarization curves were obtained
with a potential scan rate of 0.050 V / min in the potential range of -2.0 to 2.0 V
vs Ag / AgCl at room temperature.

In addition, two samples of Ti-6Al-4V and two samples of Ti-cp were

embedded through the metallographic embedding EM30D in bakelite (phenolic
resin), having a diameter of 30 mm and a maximum height of 20 mm. All
samples were hot embedded in black bakelite, the heating process took
approximately 15 minutes and the cooling process 10 minutes with a pressure
of 120 kg / cm2. Subsequently, the embedded samples were sanded in an
Aropol 2V-PU metallographic polisher, using silicon carbide sandpaper (220 to
1500). Then, polishing was performed with the OP-CHEM polishing cloth
(Struers) bathed in OP-S (colloidal silica) suspension.

Then, the samples undergone a chemical attack in order to reveal the

microstructure, using a Kroll solution. The samples were attacked by immersion,
for periods ranging from 30 to 120 s. After this procedure, micrographs were
obtained using a Scanning Electron Microscope (SEM) from Hitachi model
TM3000. In addition, an Opton trinocular optical microscope model TNM-08T-
PL has been used. After the preparation and metallographic analysis, Vickers
microhardness measurements were performed. A PANTEC brand, model
HR150, was used, which has a conical tip with diamond, with an angle of 136 °,
the adopted load of 0.2 kgf for an indentation time of 30 s, taking the average of
10 measurements for each sample.

3. Results and discussions

The final hardness average value of the Ti-10Mo-20Nb alloy was

approximately 238 ± 11.4 HV, the same procedure was adopted for the Ti-cp
and Ti-6Al-4V samples and displayed the values of 170 ± 19 HV respectively
and 340 ± 24 HV. This occurs since, the addition of the element Mo, the alloy
has a tendency to increase the value of mechanical strength (LI et al., 2020), in
addition even with a higher Nb content that acts by decreasing the hardness
value, due to be a stabilizer of the β phase preventing the formation of other
phases that increase hardness, such as α' (hexagonal martensite), α'
(orthorhombic martensite) and ω (omega phase) (BAHL et al., 2020; COSSÚ et
al., 2019). Which explains the hardness reduction behavior when compared to
Ti-6Al-4V alloy.
 The average hardness values found in the tests of the Ti-10Mo-20Nb, Ti-
cp and Ti-6Al-4V materials were compared with the hardness values of different
regions of the femur bone of a 75-year-old male donor, according to a study by
Zysset and collaborators (1999). The areas were divided and named as follows:
Osteonal femoral diaphysis (OFD), Lamellar interstitial femoral diaphysis
(LIFD), Osteonal femoral neck (OFN), Lamellar interstitial femoral neck (LIFN),
Lamellar trabecular femoral neck (LTFN). In addition to these regions, a general
average was performed, being referred to as Femoral Average (FA). Which the
corresponding value is 57.10 ± 19.6 HV.

According to Figure 1, it is evident that the Ti-6Al-4V alloy is the one with
the highest Vickers hardness and the Ti-cp alloy is closest to the bone
hardness. The hardness value of the Ti-10Mo-20Nb alloy (238 ± 11.4 HV) have
been shown to be intermediate between the two alloys, its value being 30%
lower than the Ti-6Al-4V (340 ± 24 HV) but still 4.16 times greater than the FA
(57.10 ± 19.6 HV). This reduction in hardness tends to imply a lower
maintenance rate of the implants compared to the current most used alloy of Ti-
6Al-4V, helping to reduce the effects of stress shielding (JOSHI et al., 2000;
SUL, 2003).

Figure 1: Vickers Hardness value of the respective materials (ZYSSET et al., 1999).
 The values of the elastic modulus of different regions of a human femur
from a 75-year-old male donor were also compiled (ZYSSET et al., 1999). The
values of the elastic modulus of the samples Ti-10Mo-20Nb, Ti-cp and Ti-6Al-
4V were obtained, as shown in Figure 2. Where, the corresponding average
values, respectively, of 74 ± 4 GPa, 113.5 ± 10.5 GPa and 112.5 ± 7.5 GPa.
These values were compared with the values of the elastic modulus of some
regions of a femoral bone, whose femoral average is approximately 15.68 ± 4.4
GPa (ZYSSET et al., 1999).

Figure 2: Elastic modulus of the materials (ZYSSET et al., 1999).

 Figure 3: Hardness ratio per elastic modulus of the materials (ZYSSET et al., 1999).

The Ti-cp and Ti-6Al-4V alloys have the highest elastic modulus, 112.5 ±
7.5 GPa and 113.5 ± 10.5 GPa respectively. Ti-10Mo-20Nb, on the other hand,
is closer to the elastic modulus of the bones (74 ± 4 GPa) being obtained
against the value of 15.68 ± 4.4 GPa for the bones. The decay in the average
value of the Ti-10Mo-20Nb alloy is justified by the alloy elements Nb and Mo
which tend to decrease the elastic modulus as the percentage content of the
two elements tend to increase (COSSÚ et al., 2019; LI et al., 2020). It is more
interesting that the required value of the elastic modulus is as close as possible
to the bones in order, as well as the hardness, to mitigate the effects of stress
shielding (JOSHI et al., 2000; SUL, 2003). The value of the elastic modulus
present in the Ti-10Mo-20Nb alloy was approximately 4.4 times greater than the
average of the bone values, but still 35% less than the average of the other two
alloys. This decrease in the elastic modulus together with a more adequate
hardness, tend to cause a lower rate of maintenance of the implants compared
to the currently most used alloy of Ti-6Al-4V (RACK et al., 2006; XU et al.,
2020).

The hardness ratio per elastic modulus is an important parameter to

evaluate the application for biocompatibility, in general the closer the value is to
the bones, the better are the possible applications and the mechanical behavior
is closer to the bones that will cause a reduction in the stress shielding effect
(JOSHI et al., 2000; SUL, 2003). The hardness ratio per bone elastic modulus
for the different areas of the femur bone lead to a femoral average value of
3.64, according to Zysset (1999). As shown in Figure 3, the alloy with the
highest hardness / elastic modulus ratio is the TI-10Mo-20Nb with a value of
3.22, although the Ti-6Al-4V (3.02) alloy has a very close value, only 6.62%
lower. Which indicates that both alloys are better for this type of application than
Ti-cp, whose ratio of hardness and modulus is much lower (Gabriel et al.,
2015). The Ti-10Mo-20Nb alloy (3.22) has a hardness ratio per elastic modulus
only 13% lower than the femoral average (3.64). Therefore, being an excellent
alternative for replacement and with a reduced stress shielding effect. In
addition, the Ti 6Al-4V alloy has elements that are cytotoxic, causing damage to
the health of the implant user (KRÖGER et al., 1998).

From the values found in Table 1 it was evident that the Ti-6Al-4V alloy
present the best results in corrosion resistance. Even so, the difference
between the three alloys in these aspects is small, and all three are very
resistant to corrosion in biological environment. The figure 4 even indicates the
formation of an oxide film of a passive layer on Ti-cp and Ti-10Mo-20Nb, the Ti-
cp layer being the most notable followed by Ti-10Mo-20Nb. This occurs due to
the addition of Nb instead of V, because it stabilizes the oxide layer, responsible
for the corrosion resistance of the material and passivation (KAUR et al., 2019;
ALMEIDA et al., 2014).

Table 1: Current density and corrosion potential.

Materials Ecorr. (V) Icorr. (A/cm²)

Ti – 6Al – 4V - 0.32 2.89 x 10-8
Ti-cp - 0.65 7.87 x 10-7
Ti – 10Mo – 20Nb - 0.40 7.91 x 10-6
 Figure 4: Linear polarization curve of Ti-10Mo-20Nb, Ti-cp and Ti-6Al-4V alloys.

In Figure 4, it is visible that the passivation layer, as well as the

characteristics of corrosion potential and current density of the Ti-10Mo-20Nb
alloy present slightly worst results than the Ti-6Al-4V alloy, however, it is
suitable for biological applications. In addition, it is a fact that the alloy elements
Mo and Nb are non-cytotoxic elements (KURODA et al., 1998; MORAES et al.,
2014; QAZI et al., 2005), if their ions are released by physical wear or corrosion,
they will not cause damage to the health of implant users.
 The figure 5 shows the microstructure obtained in a Ti-cp optical
microscope and the figure 6 shows the SEM micrographs of the same material.
The alloy structure appears to be heterogeneous, being formed by only two
phases, the typical Widmanstätten microstructure, where the white acicular
plates represent the α phase (HC) and the thin black lines indicate the β phase
(CCC), as well as other studies also declare (GANJEH et al., 2013).

Figure 5: OM of Ti-cp having a magnification of (a) 200X e (b) 400X.

Figure 6: Microstructure of the Ti-cp analyzed by SEM having a magnification of (a) 1500X e (b)
2000X.
 The figure 7 shows the microstructure obtained in an optical microscope
of the Ti-10Mo-20Nb alloy and the Figure 8 demonstrates as SEM micrographs
of the same alloy. It is possible to observe that a microstructure of the alloy is
basically composed of the β phase, and that it does not have a typical
Widmanstätten microstructure found in the Ti-6Al-V and Ti-cp alloys, this occurs
because the addition of Mo inhibits the transition of α phase and stabilizes the β
phase in Ti-Mo-Nb alloys. The same behavior occurs for Ti-xMo-Nb alloys of
various Mo contents (LI et al., 2020; Gabriel et al., 2008).

Figure 7: OM of Ti-10Mo-20Nb alloy having a magnification of (a) 200X e (b) 400X.

Figure 8: Microstructure of the Ti-10Mo-20Nb alloy analyzed by SEM having a magnification of

(a) 1000X e (b) 2000X.

4. Conclusion
 In the present work, Vickers microhardness, linear polarization curve, stress
shielding effect and a morphological characterization were investigated for the
Ti-10Mo-20Nb. The main conclusions are:

 The hardness value of the Ti-10Mo-20Nb alloy is 30% lower than the
Ti-6Al-4V and the value of the elastic modulus present in the Ti-
10Mo-20Nb alloy was approximately 4.4 times greater than the
average of the bone values, but still 35% less than the average of the
other two alloys. This decrease in the elastic modulus as well as with
a more suitable hardness, tend to a lower rate of maintenance of the
implants compared to the currently most used alloy of Ti-6Al-4V.

 The Ti-10Mo-20Nb alloy has a hardness ratio per elastic modulus

only 13% lower than the femoral average and 6.62% higher than Ti-
6Al-4V. Therefore, being an outstanding alternative for replacement
and with reduced stress shielding effect.

 All three alloys have good corrosion resistance, but this sample of
the Ti-6Al-4V alloy showed better corrosion resistance than Ti-10Mo-20Nb
and Ti-cp. However, the addition of Nb and Mo instead of V and Al,
improving the biocombatibility of the Ti alloy, since it stabilizes the oxide
layer, responsible for the passivation layer. In addition, it is a fact that the
alloy elements Mo and Nb are non-cytotoxic elements, being a better
alternative than Ti-6Al-4V that can cause damage to the health of implant
users.

 In Ti-10Mo-20Nb alloy is possible to observe that a microstructure

of the alloy is practically composed only of the β phase, and that it does not
have a typical Widmanstätten microstructure found in the Ti-6Al-V and Ti-cp
alloys, this possible occurs because the addition of Mo inhibits the transition
of α phase and stabilizes the β phase in Ti-Mo-Nb alloys.

Acknowledgments
 The authors wish to thank the support to this investigation by the
Brazilian agencies: CNPq, CAPES, FAPERJ for the funding.

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