Journal of Alloys and Compounds 479 (2009) 699703

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Journal of Alloys and Compounds
j our nal homepage: www. el sevi er . com/ l ocat e/ j al l com
Electrochemical characterization of -Ti alloy in Ringers solution for
implant application
Satendra Kumar

, T.S.N. Sankara Narayanan

National Metallurgical Laboratory, Madras Centre CSIR Complex, Taramani, Chennai 600 113, India
a r t i c l e i n f o
Article history:
Received 16 June 2008
Received in revised form 6 January 2009
Accepted 15 January 2009
Available online 20 February 2009
Keywords:
Titanium alloys
Corrosion behaviour
X-ray diffraction
Electrochemical characterization
Biomedical applications
a b s t r a c t
The corrosion behaviour of Ti15Mo alloy in Ringers solution was evaluated by potentiodynamic polar-
ization, cyclic polarization and chronoamperometric/currenttime transient (CTT) studies. The corrosion
protective ability of Ti15Mo alloy was compared with that of commercially pure (CP) titanium (grade-
2) and Ti6Al4V alloy under similar experimental conditions. The microstructure, microhardness and
structural characteristics werealsoevaluatedtoascertainthesuitabilityof thesematerials for orthopaedic
implant applications. The study reveals that Ti15Mo alloy possesses a -phase microstructure and
moderate hardness. The open circuit potential of Ti15Mo alloy is relatively nobler than CPTi and
Ti6Al4V alloy. The average passive current density of all the three Ti materials studied lies in the range
of 3210
6
A/cm
2
. The passivation range of Ti15Mo alloy is relatively large when compared to that of
Ti6Al4V alloy and CPTi. The loop area of the cyclic polarization curve of Ti15Mo alloy is quite similar
to that of Ti6Al4V alloy but relatively smaller than that of CPTi. There is no appreciable variation in
the steady state current density of all the three Ti materials measured at +0.5V vs. SCE whereas a signi-
cant variation is observed at +1.25V vs. SCE. Based on the -phase structure, moderate hardness and the
ability to offer a better corrosion resistance in Ringers solution, Ti15Mo alloy can be used as a suitable
alternative material for orthopaedic implant applications.
2009 Elsevier B.V. All rights reserved.
1. Introduction
Titaniumandtitaniumalloys are widely usedfor many biomedi-
cal applications due to their lowdensity, excellent biocompatibility,
corrosion resistance and mechanical properties [14]. Among the
various types of Ti alloys, Ti6Al4V alloy has been the choice
in many instances. However, studies have expressed concerns
on the use of this alloy in spite of the fact that the mechanical
properties and corrosion resistance of Ti6Al4V alloy are ideal for
implant applications. The two major concerns are: (i) the leaching
of V and Al that could cause long term health problems such
as peripheral neuropathy, osteomalacia and Alzheimer diseases
[5]; and (ii) the large modulus mismatch between the Ti6Al4V
alloy (110GPa) and the bone (1040GPa), which could cause
insufcient loading on bone adjacent to the implant, leading to an
eventual failure of the implant [6]. The high modulus of Ti6Al4V
alloys is attributable to the high volume fraction of the -phase
in them. Since the -phase in Ti alloys exhibits a signicantly
lower modulus than the -phase, development of lower modulus

Corresponding authors. Tel.: +91 44 2254 2077; fax: +91 44 2254 1027.
E-mail addresses: sat nml@rediffmail.com (S. Kumar), tsnsn@rediffmail.com
(T.S.N. Sankara Narayanan).
-Ti alloys, which retain a single -phase microstructure on rapid
cooling from high temperatures, assumes signicance. Several
-phase Ti alloys, using Nb, Ta and Mo as alloying elements
(-stabilizers), such as Ti12Mo6Zr2Fe, Ti13Mo7Zr3Fe
(TMZF), Ti15Mo5Zr3Al, Ti15Mo3Nb3O (TIMETAL 21Srx),
Ti14Nb13Zr, Ti35Nb7Zr5Ta, Ti34Nb9Zr8Ta (TNZT),
Ti29Nb4.6Zr13Ta, Ti15Mo, Ti12Mo5Ta, Ti25Nb3Fe, etc.
[612] were developed.
Ho et al. [6], Nag et al. [13], Ho [14] and Oliveira et al. [15] have
studiedthestructureandproperties of aseries of binaryTiMoalloy
with Mo content ranging up to 20wt.%. Based on the microstruc-
tural evolution and strengthening mechanisms, Nag et al. [13] have
recommended Ti15Mo alloy as one of the promising biocompat-
ible Ti alloy. The corrosion behaviour of TiMo alloys in simulated
body uid and dental environment was studied earlier [1522].
Oliveira et al. [15] have evaluatedthe corrosionbehaviour of a series
of TiMo alloys with 420wt.% Mo content in Ringers solution.
AccordingtothemincreaseinMocontent of theTiMoalloyenables
an improvement in the corrosion protective ability. Oliveira et al.
[15] and Oliveira and Guastaldi [19,20] have reported that TiMo
alloys having 420wt.% Mo exhibit spontaneous passivation in
Ringers solutionand do not exhibit pitting evenat very highpoten-
tials, upto8V(vs. SCE). Basedontheir abilitytoexhibit spontaneous
passivation, electrochemical stability of the passive lms and bet-
0925-8388/$ see front matter 2009 Elsevier B.V. All rights reserved.
doi:10.1016/j.jallcom.2009.01.036
700 S. Kumar, T.S.N. Sankara Narayanan / Journal of Alloys and Compounds 479 (2009) 699703
Table 1
Chemical composition of the Ti materials used in this study.
Element CPTi (grade 2) Ti6Al4V alloy Ti15Mo alloy
N 0.01 0.02 0.01
C 0.03 0.03 0.02
H 0.010 0.011 0.011
Fe 0.20 0.22 0.012
O 0.18 0.16 0.10
Al 6.12
V 3.93
Mo 15.04
Ti Balance Balance Balance
ter biocompatibility, Oliveira and Guastaldi [19,20] have suggested
that TiMo alloys can be used as a biomaterial. Alves et al. [17]
have evaluated the corrosion resistance of Ti10Mo alloy in uori-
dated physiological serum (0.15M NaCl +0.03M NaF [pH=6]) and
compared with that of Ti6Al4V alloy. The corrosion behaviour of
Ti15Mo alloy in 0.15M NaCl solution containing varying concen-
trations of uoride ions (190, 570, 1140 and 9500ppm) was studied
recently by Kumar and Sankara Narayanan [18] for dental implant
applications. Karthega et al. [21] have reported that the corrosion
resistance of Ti15Mo and Ti29Nb13Ta4.6Zr (TNTZ) (titanium
alloys) in Hanks solution are almost similar. Based on the corrosion
protective ability Capela et al. [22] have ranked the TiMo alloys as
follows: CPTi >Ti6.5Mo>Ti8.5Mo>Ti10Mo. The present study
aims to evaluate the corrosion resistance behaviour of Ti15Mo
alloy in Ringers solution and, to compare its corrosion protective
ability with that of commercially pure (CP) titanium (grade 2) and
Ti6Al4V alloy under similar conditions, to ascertain the suitabil-
ity of Ti15Mo alloy for orthopaedic implant applications.
2. Experimental details
Commercially pure titanium (grade 2) and, Ti6Al4V and Ti15Mo alloys were
used in this study. The chemical composition of these Ti materials is given in Table 1.
For microstructural evaluation, the Ti materials were mechanically polished using
various grades of SiC paper and nally using a 0.3-m diamond paste. The polished
specimens were then etched using a HNO3
HF mixture (15vol.% HNO
3
; 5vol.% HF;
80vol.%water) for 30s, rinsed in deionized water and dried. The microstructure of Ti
materials was examinedusingaLeicaDMLMoptical microscopewithimageanalyzer
software. The structural characteristics of the three Ti materials were evaluated by
X-ray diffraction (XRD) measurement. The hardness of Ti materials was determined
using a Leica VMHTMOT microhardness tester with a Vickers diamond indenter
under a load of 200g. The lap time for each indentation was 15s and the values
reported represent the average of ve measurements.
The corrosion behaviour of CPTi, Ti6Al4V and Ti15Mo alloys was studied by
potentiodynamic polarization, cyclic polarization and chronoamperometric/
currenttime transient (CTT) studies usinga Potentiostat/Galvanostat of ACMinstru-
ments (Model: Gill AC) and a at cell (Wear and Friction Tech, Chennai, India).
Ringers solution having a chemical composition (in g/l) of 9 NaCl, 0.24 CaCl2
, 0.43
KCl and 0.2 NaHCO
3
(pH: 7.8) [23] in non de-aerated condition was used as the
electrolyte. Before conducting the corrosion studies, all the three Ti materials were
mechanically polished using various grades of SiC paper, rinsed with deionized
water, pickled using a HNO
3
HF mixture (35vol.% HNO
3
; 5vol.% HF; 40vol.% water)
at 40

C for 6070s [24], rinsed in deionized water and dried using a streamof com-
pressed air. The cleaned Ti samples were placed inside a at cell so that only 1cm
2
area of the sample was exposed to the Ringers solution. The Ti samples forms the
working electrode. A saturated calomel electrode (SCE) and a graphite rod were
used as the reference and counter electrodes, respectively. All experiments were
conducted at 371

C.
Before conducting the potentiodynamic or cyclic polarization studies, the three
Ti materials were immersed in Ringers solution for 1h for stabilization and their
open circuit potentials (OCP) were measured during this period. Potentiodynamic
polarization tests were performed at a scan rate of 100mV/min. Both in the cathodic
and anodic directions, from their respective open circuit potential. In the cathodic
direction, the potential scan was limited to 250mV whereas in the anodic direction
the potential was scanned up to 3000mV fromtheir respective OCP. Cyclic polariza-
tion study in Ringers solution was also performed to compare the pitting corrosion
resistance of all three Ti materials used in present study. During cyclic polarization
study, the potential of the samples was reversed after reaching an anodic potential
of +2000mV vs. SCE with respect to their respective OCP. CTT studies of all the three
Ti materials in Ringers solution were performed at +0.50 and +1.25V vs. SCE for the
time duration of 90min. The potentiodynamic polarization, cyclic polarization and
CTT studies were repeated at least three times so as to ensure reproducibility of test
results.
3. Results and discussion
3.1. Microstructure
The microstructure of CPTi, Ti6Al4V and Ti15Mo alloys are
shown in Fig. 1(a)(c), respectively. The microstructure of CPTi
(Fig. 1(a)) exhibits a typical rapidly cooled metastable feather-
like microstructure that consists of equiaxed -grain with some
twin bands. The microstructure of Ti6Al4Vreveals structure
(Fig. 1(b)) that consists of elongated -grains (light) and inter-
granular -grains (mottled or outlined). In case of Ti15Mo alloy
(Fig. 1(c)) equiaxed -grains is observed as the dominant phase.
The grains are homogeneous and evenly distributed. Ho et al. [6]
have reported that TiMo alloys having 9wt.% Mo have a signi-
cant amount of equiaxed -phase and in alloys containing 10wt.%
Mo; the -phase became the only dominant phase. Davis et al. [25]
have also suggested the retention of -phase at higher Mo content.
Bania [26] has reported that a minimum of 10wt.% Mo is required
to fully stabilize the -phase at roomtemperature. The presence of
15wt.% Mo makes the -phase as the only dominant phase in the
microstructure of the Ti15Mo alloy (Fig. 1(c)) and supports the
observations made by other researchers [6,25,26].
3.2. Structural characteristics
The X-ray diffraction pattern of CPTi, Ti6Al4V and Ti15Mo
alloys areshowninFig. 2(a)(c), respectively. It is evident fromFig. 2
that the XRDpatternof CPTi is comprisedentirely of hexagonal

-
phase; the Ti15Mo alloy exhibits the presence of only the -phase
whereas the Ti6Al4V alloy exhibits the presence of both - and
Fig. 1. Microstructure of the Ti alloys: (a) CPTi; (b) Ti6Al4V alloy; and (c) Ti15Mo alloy.
S. Kumar, T.S.N. Sankara Narayanan / Journal of Alloys and Compounds 479 (2009) 699703 701
Fig. 2. X-ray diffraction pattern of the Ti alloys: (a) CPTi; (b) Ti6Al4V alloy; and
(c) Ti15Mo alloy.
-phases. The presence of only the -phase for TiMo alloys having
10wt.% Mo has also been reported earlier by Ho et al. [6].
3.3. Microhardness
The average microhardness of CPTi, Ti6Al4V and Ti15Mo
alloys is found to be 175, 324 and 238HV
0.2
, respectively and they
are in agreement with the values reported elsewhere [6,13,27,28].
Among them, the -phase CPTi has the lowest microhardness and
the Ti6Al4V alloy with + phase posses the highest hardness
whilethehardness of Ti15Moalloylies inbetweenthesetwo. Hoet
al. [6] have reported that the hardness of CPTi (156HV) is far less
than that of Ti12.5Mo alloy (340HV). Okasaki [28] has reported
that the hardness of CPTi, Ti6Al4V and Ti15Zr4Nb4Ta alloys
(-phase Ti alloy) are in the range of 180, 340 and 330HV,
respectively. Gordin et al. [11] have reported that the hardness
of Ti6Al4V and Ti12Mo5Ta alloys (-phase Ti alloy) are 330
and 303HV, respectively. However, the hardness of Ti20Mo alloy
is found be higher than that of Ti6Al4V alloy [6]. Based on the
hardness values reported in the literature and the values obtained
in the present study, it is clear that the hardness of TiMo alloys is
higher than that of CPTi. However, compared to Ti6Al4V alloy,
the hardness of TiMo alloys appears to be inuenced by the Mo
content. As several factors might inuence the microhardness of the
TiMoalloys, whichinclude solidsolutionstrengthening, precipita-
tion hardening, strain aging, grain size and crystal structure/phase
Fig. 3. Potentiodynamic polarizationcurves of CPTi, Ti6Al4Vand Ti15Mo alloys
in Ringers solution (scan rate: 100mV/min) (potential in mV vs. SCE).
Table 2
Passivation range, passive current density and pitting potentials of CPTi, Ti6Al4V
and Ti15Mo materials in Ringers solution.
Type of Ti sample used Passivation range
(mV) vs. SCE
Passive current density
(110
6
A/cm
2
)
CPTi grade 2 1451522 32.0
Ti6Al4V alloy 1561460 32.4
Ti15Mo alloy 1662513 32.4
(, +, ) [6], predicting the extent of change in hardness only
with the extent of Mo alloying is difcult.
3.4. Electrochemical characterization
3.4.1. Open circuit potential measurement
TheTi samples wereimmersedinRingers solutionfor 1hfor sta-
bilization and the open circuit potential was measured during this
period. The OCP of CPTi and Ti6Al4V alloy is almost the similar,
520 and 516mV vs. SCE, respectively, while the OCP of Ti15Mo
alloy is 477mVvs. SCE. The relatively nobler OCP of Ti15Mo alloy
indicates that it could offer a better corrosion resistance in Ringers
solution than CPTi and Ti6Al4V alloy. To get a better in sight
about the electrochemical corrosion behaviour of the Ti samples in
Ringers solution, potentiodynamic polarization, cyclic polarization
and chronoamperometric studies were performed.
3.4.2. Potentiodynamic polarization studies
The potentiodynamic polarization curves of CPTi, Ti6Al4V
and Ti15Mo alloys in Ringers solution, shown in Fig. 3, are quite
similar. The anodic branchof the curves showa passive regionasso-
ciated with the formation of one or more protective lms. For a
clear analysis, the anodic portion of the curve is divided into two
segments; the potential region from 300 to +1200mV vs. SCE as
segment I whereas the potential region above +1200mV vs. SCE as
segment II. In segment I, passive current densities of all the three
Ti materials are notably less whereas in segment II the passive cur-
rent densities are relatively higher. In segment I, the polarization
curves of CPTi and Ti6Al4V alloy overlap each other and their
passivecurrent densities arequitesimilar. However, thepassivecur-
rent density of Ti15Mo alloy is relatively lower in this segment.
Though segment II does not represent a clinical reality and there
could be a possible decomposition of the electrolyte, this segment
is considered here only to compare the range of passivation of the
three Ti materials in Ringers solution. The passivation range and
average passive current density of CPTi, Ti6Al4V and Ti15Mo
alloys are compiled in Table 2. The passivation range of Ti15Mo
alloy(1662513mVvs. SCE) is relativelylarger thanTi6Al4Valloy
(1551460mV vs. SCE) and CPTi (1451522mV vs. SCE). The aver-
age passive current density of all the three Ti materials lies is in
the range of 3210
6
A/cm
2
. The surface morphology of CPTi,
Ti6Al4V and Ti15Mo alloys after subjecting them to polariza-
tion studies indicate that their surface is free from pits. Alkhateeb
and Virtanen [29] have also reported that no signs of localized cor-
rosion attack on the surface of CPTi (grade 2) after the polarization
studies.
3.4.3. Cyclic polarization studies
The cyclic polarization plots of CPTi, Ti6Al4V and Ti15Mo
alloys in Ringers solution are given in Fig. 4. The reverse scan curve
of all the three Ti materials came above the forward scan, which
indicates that, the Ti materials are resistant to pitting corrosion in
Ringers solution(Fig. 4(a) and(b) andTable3). Thepittingcorrosion
resistance of any material/coating, in general, can be ranked based
on the loop area of the cyclic polarization curves. The higher the
loop area, the poorer is the resistance to pitting corrosion and vice
702 S. Kumar, T.S.N. Sankara Narayanan / Journal of Alloys and Compounds 479 (2009) 699703
Fig. 4. Comparison of potentiodynamic polarization curves of the Ti alloys in
Ringers solution (scan rate: 100mV/min) (potentials in mV vs. SCE): (a) CPTi and
Ti15Mo alloy; and (b) Ti15Mo and Ti6Al4V alloys.
versa [30]. The loop area of all the three Ti materials studied is in
the range of (3.34.5) 10
5
C/cm
2
(Table 3). Among the three Ti
materials, the loop area is relatively lower for Ti15Mo alloy when
compared to CPTi (Fig. 4(a)) whereas the loop area of Ti15Mo
and Ti6Al4V alloys is quite similar (Fig. 4(b)). This observation
indicates that the pitting corrosion resistance of Ti15Mo alloy is
highly comparable to that of Ti6Al4V alloy but better than CPTi.
Oliveira et al. [15] have also reported that no pitting corrosion has
occurred on TiMo alloys in Ringers solution.
3.4.4. Chronoamperometric/currenttime transient studies
A chronoamperometric/currenttime transient study, which is
a measure of the change in current as a function of time at a con-
stant impressed potential, would indicate the ability of Ti and its
alloys to form a stable passive lm. Chronoamperometric studies
have been used earlier by Alves et al. [17] and, Kumar and Sankara
Table 3
Corrosion potential during the forward and reverse scans and the loop area of CPTi,
Ti6Al4V and Ti15Mo alloys in Ringers solution.
Type of Ti sample used E-1
a
(mV)
vs. SCE
E-2
a
(mV)
vs. SCE
Loop area
(C/cm
2
)
CPTi grade 2 250 213 4.510
5
Ti6Al4V alloy 479 299 3.510
5
Ti15Mo alloy 496 300 3.310
5
a
E-1 and E-2: corrosion potential during the forward and reverse scans.
Fig. 5. Currenttime transient curves of CPTi, Ti6Al4V and Ti15Mo alloys in
Ringers solution at various anodic potentials: (a) 0.5V; (b) 1.25V; (c) 2V; and (d)
3V (potentials in V vs. SCE).
Narayanan [18] to evaluate the passive state of TiMo alloys in
simulated oral environment at different anodic potentials. The CTT
curves of CPTi, Ti6Al4V and Ti15Mo alloys in Ringers solution
at +0.5 and +1.25V vs. SCE display similar characteristics; a rapid
decrease incurrent followedby a slowdecay toattaina steady state.
The observed behaviour could be explained based on the decrease
in active area due to the growth of a passive lm [17,18]. There
is no appreciable variation in the steady state current density of
all the three Ti materials measured at +0.5V vs. SCE (Fig. 5(a) and
Table 4). However, a signicant variation in the steady state current
density of all the three Ti materials is observed at +1.25V vs. SCE
and it follows the order: Ti6Al4V<CPTi <Ti15Mo (Fig. 5(b) and
Table 4). Unlike CPTi, the extent of dissolutionandre-precipitation
of the alloying elements such as Al, V and Mo would inuence the
nature of the lmthat would formon the surface of Ti6Al4V and
Ti15Mo alloys. The relatively lower current density value observed
for Ti6Al4Valloy comparedto CPTi andTi15Mo alloy at +1.25V
vs. SCE is due to the formation of Al
2
O
3
layer on its surface. The
Table 4
Steady state current density of CPTi, Ti6Al4V and Ti15Mo alloys in Ringers
solution measured at different impressed potentials.
Type of Ti sample used Steady state current density (110
6
A/cm
2
)
measured at constant impressed potential
+0.5V vs.SCE +1.25V vs. SCE
CPTi grade 2 0.26 1.54
Ti6Al4V alloy 0.32 0.99
Ti15Mo alloy 0.43 2.17
S. Kumar, T.S.N. Sankara Narayanan / Journal of Alloys and Compounds 479 (2009) 699703 703
relatively higher current density value observed for Ti15Mo alloy
indicates a possible dissolution of Mo from the alloy. However, all
the three Ti materials have the ability to quickly form a stable pas-
sive lmat +0.5 and +1.25V vs. SCE. The results of the currenttime
transient studies suggest that CPTi, Ti6Al4V and Ti15Mo
alloys possess better ability to form a stable passive lm on their
surfaces.
The potentiodynamic polarization, cyclic polarization and CTT
studies of CPTi, Ti6Al4V and Ti15Mo alloys in Ringers solu-
tion reveal that the corrosion resistance of Ti15Mo alloy is highly
comparable to that of Ti6Al4V alloy but better than that of
CPTi. Though the hardness of Ti15Mo alloy is lower than that
of Ti6Al4V alloy, being a -phase alloy the Ti15Mo alloy
is expected to offer better modulus property than CPTi and
Ti6Al4V alloy [6,13]. Besides, the absence of toxic elements such
as V and Al render Ti15Mo alloy much safer to be used in human
body. Hence, the Ti15Mo alloy that possesses a -phase struc-
ture, moderate hardness and higher corrosion resistance could be
a suitable alternative material for orthopedic implant applications.
4. Conclusions
The microstructure and structural characteristics conrm that
Ti15Mo alloy possess equiaxed -phase in it is microstructure.
The hardness of Ti15Mo alloy (238HV
0.2
) lies between that of
CPTi (175HV
0.2
) and Ti6Al4V alloy (324HV
0.2
). The OCP of CPTi
and Ti6Al4V alloy is almost the similar, 520 and 516mV vs.
SCE, respectively, while the OCP of Ti15Mo alloy is 477mV vs.
SCE. Potentiodynamic polarization curves of CPTi, Ti6Al4V and
Ti15Mo alloys in Ringers solution are quite similar. The aver-
age passive current density of all the three Ti materials lies is
in the range of 3210
6
A/cm
2
. However, the passivation range
of Ti15Mo alloy (1662513mV vs. SCE) is relatively larger than
Ti6Al4V alloy (1551460mV vs. SCE) and CPTi (1451522mV
vs. SCE). The loop area of the cyclic polarization curve of Ti15Mo
alloy is quite similar to that of Ti6Al4Valloy but smaller thanthat
of CPTi. There is no appreciable variation in the steady state cur-
rent density of all the three Ti materials measured at +0.5V vs. SCE
while a signicant variation is observed at +1.25V vs. SCE. All the
three Ti materials have the ability to quickly form a stable passive
lm in Ringers solution at +0.5 and +1.25V vs. SCE. The -phase
structure, moderate hardness and the ability to offer a better cor-
rosion resistance in Ringers solution enables Ti15Mo alloy as a
suitable alternative material for orthopedic implant applications.
Acknowledgement
The authors express their sincere thanks to Prof. S.P. Mehro-
tra, Director, National Metallurgical Laboratory, Jamshedpur, for his
keen interest and permission to publish this paper.
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