M A TE RI A L S C HA RACT ER I ZA TI O N 84 ( 20 1 3 ) 1 0 51 1 1

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Microstructure and beta grain growth behavior of

TiMo alloys solution treated
Jin-Wen Lua,b,, Yong-Qing Zhaoa,b,, Peng Geb , Hong-Zhi Niub
a

School of Materials and Metallurgy, Northeastern University, Shenyang 110819, China

Northwest Institute for Nonferrous Metal Research, Xi'an 710016, China

AR TIC LE D ATA

ABSTR ACT

Article history:

The microstructure and grain growth kinetics of TiMo binary alloys in the phase have

Received 5 November 2012

been studied. The results show that the phase composition and grain growth kinetics of the

Received in revised form 15 July 2013

solution-treated alloys are sensitive to Mo content. Ti1Mo alloy mainly containes

Accepted 22 July 2013

hexagonal phase, while Ti4Mo alloy is composed of dominated phase and some
inner acicular . When Mo content increases to 10 wt% or higher, the retained phase

Keywords:

becomes the only phase. The grain size is not only related to temperature and solution

TiMo alloys

time, but also relates to Mo content. The grain growth rate of Ti4Mo alloy during solution

Microstructure

treatment is much faster than that of Ti20Mo alloy, and the time exponent 0.42 of the Ti

Solution treatment

4Mo alloy is higher than that of Ti20Mo alloy due to the low dislocation density. However,

Grain growth

the grain-growth activation energy of Ti20Mo alloy is 272.16 kJ/mol, which is much higher

Tensile properties

than that of Ti4Mo alloy, due to the solute drag effect of Mo. The room-temperature
strength and plasticity of TiMo alloys increase with the increasing of Mo content and
decreasing of grain size.
2013 Elsevier Inc. All rights reserved.

1.

Introduction

Titanium and titanium alloys, with high specific strength,

high corrosion resistance, low elastic modulus and excellent
biocompatibility, are extensively used in aerospace, petrochemical and biomedical industries [15]. Because of the
releasing of toxicity of V and Al icons from the Ti6Al4 V
alloy, the latest research activities are oriented to titanium
alloys composed of non-toxic elements [68]. Mo is one of the
elements which have been judged to be non-toxic and
non-allergic, and it has been selected as one of the safe
alloying elements to develop low elastic modulus titanium
alloys with high strength for biomaterials. It is also well
known that Mo has high phase stabilization effect and is
able to form the infinite solid solution in -Ti [9,10]. Alloyed by
element Mo, the -transus temperature of titanium alloy is
decreased, and the properties such as strength, corrosion
resistance, high-temperature performance and formability

can be improved [11]. Therefore, it plays an important role in

titanium alloys designed for biomedical application.
A small grain size of structural alloy is usually required to
optimize the strength and plasticity, so that a good understanding of grain growth is a prerequisite for controlling the
microstructure and properties of titanium alloy [12,13]. It is
well known that the driving force for grain growth is the
reduction of the free energy associated with the decreasing of
the grain boundary area [14]. Grain growth takes place by
diffusion, when the temperature is high enough and the time of
solution treatment is long enough. The mechanism of grain
growth process includes the normal grain growth and abnormal
grain growth or secondary recrystallization. There have been at
least two different types of approaches to study grain growth
behavior by now. The first one emphasizes the research of grain
growth kinetics by measuring average grain size of the whole
samples in the micrograph, and the other researches the
features of microstructural morphology by using the advanced

Corresponding authors at: No.96 Weiyang Road, Xi'an, Shaanxi 710016, P.R.China. Tel.: + 86 29 86231078; fax: +86 29 86360416.
E-mail addresses: lujwen@163.com (J.-W. Lu), trc@c-nin.com (Y.-Q. Zhao).
1044-5803/$ see front matter 2013 Elsevier Inc. All rights reserved.
http://dx.doi.org/10.1016/j.matchar.2013.07.014

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M A TE RI A L S CH A RACT ER IZ A TI O N 84 (2 0 1 3 ) 1 0 51 1 1

Table 1 Mo content of experimental TiMo alloys (mass

%).
Alloy
Mo contents

Ti1Mo Ti2Mo Ti4Mo Ti15Mo Ti20Mo

1.15

2.15

3.96

14.11

20.30

measuring equipments and analysis techniques [15]. Over the

past few decades, the microstructure and mechanical property
of the TiMo alloys have been investigated by many scientists
all over the world. Ho [16] and Oliveira et al. [17,18] have studied
microstructures and properties of cast binary TiMo alloys, and
the cold-rolled TiMo alloys for dentistry have been investigated by Chen et al. [19] and Zhou et al. [20,21]. Furuhara's [22]
result showed that precipitate was formed in the matrix in
the Ti10, 20 and 30 Mo alloys (wt%), and grew into the interior
of grains at the aging temperature range between 923 K and
773 K. Nevertheless, little attention has been paid to the
influence of Mo contents on the grain growth process of TiMo
alloys, so it is necessary to understand the relationship between
the grain growth and the mechanical property.
In the present study, the microstructure and kinetics of
grain growth in TiMo binary alloys after solution treatment
with different Mo contents are analyzed, and the influence of
the grain size on the mechanical properties have been also
investigated. The aim of this work is to understand the
mechanism of the beta grain growth behavior with increasing
the Mo contents, and to provide experimental evidence for the
role of alloying element Mo in titanium alloy design.

2.

Materials and Experimental Procedure

The Mo content of TiMo alloys selected for this study include 1,

2, 4, 15 and 20 wt% and the kinetics of grain growth was studied
in phase of the Ti4Mo and Ti20Mo alloys. All the materials
were prepared from raw titanium (99.9% pure) and molybdenum (99.9% pure) using a commercial arc-melting vacuum
pressure casting system. The melting chamber was firstly
evacuated and then purged with argon. An argon pressure of
1.5 kgf/cm2 was maintained during melting process. Appropriate amounts of each kind of the metal were melted in a
U-shaped copper hearth with a tungsten electrode. All the
alloys were re-melted three times at 1273 K for 10.8 ks to
improve the chemical homogeneity and then given around 60%
reduction by hot-forging into quadrate blocks of 70 mm
wide 30 mm thick 600 mm length followed by air cooling.
The actual chemical compositions were determined by energy
dispersive spectrometry, and the results are listed in Table 1.

The -transus temperatures of the tested Ti4Mo and Ti20Mo

alloys were identified by solution treating specimens in the
temperature range of 650 ~ 900 C and examining the microstructure (metallographic techniques), and their -transus
temperatures were found to be 865 and 710 C, respectively.
Cubic specimens (10 mm 10 mm 10 mm) were spark machined from the quadrate blocks, then were placed in the argon
atmosphere in the tubular furnace to perform different heat
treatments (Table 2). The specimens after solution treatment
were removed from the furnace according to the time sequence
and then quenched in air.
The specimens were then grounded, polished, and etched in
solution composed of 5 vol.% HF, 10 vol.% HNO3, and 85
vol.%H2O. X-ray diffraction for phase analysis was conducted
on Rigaku diffractometer (Rigaku D-max IIIV, Rigaku Co., Tokyo,
Japan) in the typical 2 range of 2090 and operated at 30 kV and
200 mA, The phase was identified by matching each characteristic peak with JCPDS files. Moreover, the dislocation density of
the initial states of the TiMo alloys was also determined using
X-ray diffractometry according to the equation of Dunn[23]. The
dislocation density for Ti4Mo and Ti20Mo alloys before solution
treatment was 1.05 1014 and 2.64 1014 m2, respectively. The
microstructures of TiMo alloys were observed on the optical
microscopy (OM, OLYMPUS GX71) and the grain size was
calculated by the Metal-methods for estimating the average
grain size (Planimetry, GB/T 6394-2002, CHINA). Tensile specimens with a gage length of 40 mm and a cross section of 5 mm in
diameter were fabricated by machining from these prestrained
and heat-treated specimens after removal of surface oxides.
Uniaxial tensile tests were carried out at a cross-head speed of
1 mm/min1 at room temperature. The ultimate tensile strength,
yield strength, elongation and the area of reduction at fracture
were accordingly determined.

3.

Results and Discussion

3.1.

Microstructures

The results obtained in this work show that the phase

composition of the binary TiMo alloys were sensitive to Mo
content. As shown in Fig. 1, Ti1Mo alloy mainly contains
hexagonal phase, while the solution treated (ST) Ti4Mo alloy
is composed of dominated phase and some . When Mo
content increases to 10 wt% or higher (15 and 20 wt%), the
retained phase becomes the only phase. However, there are
little peaks of phase at 35 and 40 in X-ray diffraction profiles
of the Ti15Mo alloy, this is main because that the solution

Table 2 Heat treatment temperatures and times.

Material

Phase

Temperatures (C)

Times (min)

Ti1Mo
Ti2Mo
Ti4Mo
Ti15Mo
Ti20Mo

900
900
900, 950, 1000, 1050
800
650, 700, 750, 800,900

60
60
15, 30, 60, 120, 240, 360
60
15, 30, 60, 120, 240, 360

Cooling-down method
Air cooling

M A TE RI A L S C HA RACT ER I ZA TI O N 84 ( 20 1 3 ) 1 0 51 1 1

107

Fig. 1 X-ray diffraction profiles of the TiMo alloy after

solution treatment.

treated temperature of Ti15Mo alloy (800 C) approaches to its

-transus temperatures 795 C and phase needs enough time
or higher temperature for phase transformation.
The microstructure of the series ST TiMo alloys, as shown
in Fig. 2, are nearly consistent with the XRD results. The ST Ti
1Mo exhibits a typical equiaxed phase microstructure. When
Mo content is 4 wt%, the fine, acicular martensitic structure of
phase and the retained phase can be observed. When the
alloy contains 10 wt% or more Mo (15 and 20 wt%), equiaxed
phase becomes the only phase.
Similar results were found by Zhou et al. [20,21], Ho et al.
[16] and Davis et al. [24], they have analyzed the binary TiMo
alloys after solution treatment. When Mo content was 10 wt
%, a new phase except was detected and the ST Ti20Mo
alloy was composed of single phase. Ho et al. [16] proved
that a minimum of 10 % Mo was required to completely
stabilize the phase at room temperature. When the Mo
content was within the range of 4 and 10 wt%, the phase and
crystal structure of the ST TiMo alloys were sensitive to the
Mo concentration and solution temperature. Davis et al. [24]
has reported that, in the cast TiMo system, the martensitic
structure changed from hexagonal () to orthorhombic () at
around 6 wt% Mo. Those studies have an exceedingly important effect for us to understand the phase transformation and
the mechanical properties of the alloy.

3.2.

Grain Growth Kinetics

In this section, the kinetics of grain growth in binary Ti4Mo

and Ti20Mo alloys was analyzed and compared. All the
grains of binary Ti4Mo and Ti20Mo alloys was equiaxed
after solution treatment. Fig. 3 presents the microstructure of
Ti4Mo alloy solution treated at 900 C for various times, Fig. 4
presents the microstructure of Ti20Mo alloy solution treated
at 800 C for various times. From Figs. 3 and 4, it can be
observed that the grains in more Mo content alloys are
much smaller than those in less Mo content alloys around 4%.
The grain size as a function of solution time is plotted in
Fig. 5 for Ti4Mo and Ti20Mo alloys. As shown, the grain size
increases with increasing the solution treatment time, and the

Fig. 2 Optical micrographs of the TiMo alloy after solution

treatment: (a) Ti1Mo, (b) Ti4Mo, (c) Ti15Mo and (d) Ti20Mo.

grain growth rate of Ti4Mo alloy is much faster than that of Ti

20Mo alloy in the same condition. It is also worth to note that
the grain growth takes place at a very fast rate in the first 15
60 min during the solution treatment, and the growth rate

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Fig. 3 Optical micrographs of the Ti4Mo alloy solution treated

at 900 C for various time: (a) 60 min, (b) 120 min, (c) 240 min
and (d) 360 min.

decreases as time goes on. This phenomenon can be explained

by the increasing of the grain size, which leads to a decrease in
the grain boundary area per unit volume. This may mean that

Fig. 4 Optical micrographs of the Ti20Mo alloy solution

treated at 800 C for various time: (a) 60 min, (b) 120 min,
(c) 240 min and (d) 360 min.

the grain boundary interfacial energy per unit volume decreases, therefore the driving force for grain growth lowers.
The grain size as a function of the time at 900 C and 800 C
is plotted logarithmically in Fig. 6 for Ti4Mo and Ti20Mo

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M A TE RI A L S C HA RACT ER I ZA TI O N 84 ( 20 1 3 ) 1 0 51 1 1

Fig. 5 Increase of the grain size in relation to solution time

in phase at 800 C (Ti20Mo) and 900 C (Ti4Mo).

alloys. Generally, the expression for grain growth can be given

by the following equation [14,15].
Dt D0 Kt n

where Dt is the average grain size, D0 is the initial grain size,

K is a temperature dependent constant, t is the time and n is the
time exponent obtained from the slope of the lnD vs. lnt plot.
The grain growth time exponent n for Ti4Mo (900 C) and Ti
20Mo (800 C) alloys is 0.42 and 0.26, respectively. It can be
concluded that the time exponent of the Ti4Mo alloy is higher
than that of Ti20Mo. The difference in growth time exponent is
mainly caused by the different solution treatment temperature
and chemical composition [25]. Ti20Mo alloy presents high
alloying element content and very high dislocation density
which causes by high Mo content during solution treatment
process, and Ti4Mo alloy possesses high purity and very low
dislocation density. For these reasons, the time exponent of Ti
20Mo alloy is lower than that of Ti4Mo alloy. In general, the
growth exponent in the kinetics of normal growth is below 0.5
due to the role played by different grain growth parameters
such as impurity-drag, free surface effect, texture, dislocation

Fig. 7 Increase of the grain size in relation to solution

temperature in phase at 60 min.
substructure and heterogeneities [24 ~ 26]. It has been reported
that the growth exponent of -Ti increases with the increasing
of solution temperature from 0.30 at 700 C to 0.45 at 800 C, and
this can be explained by the crystal structure changing from
(hexagonal) to (body centered cubic) [21].
The grain size as a function of solution temperature is
plotted in Fig. 7 for Ti4Mo and Ti20Mo alloys. It is found that
the grain size increases with the increasing of the solution
treatment temperature, and the grain growth rate of Ti4Mo
alloy is also much faster than that of Ti20Mo alloy with the
same solution time. As expected, the graph showed very rapid
grain growth up to a heat treatment temperature of 50 C above
the -transus. It is well known that the atomic diffusion across
the grain boundary is a simple thermal-activated process, the
effect of temperature on grain growth is actually the effect of
temperature on atomic diffusion crossing boundary. The grain
growth rate increases with the temperature, because the
average migration rate of grain boundary is proportional to
exp (-Q/RT). Generally, the grain growth rate under isothermal
condition can be expressed as [14,15]:
dD=dt K 1 D1 eQ =RT

where K1 is a constant, Q is the activation energy of grain growth

obtained from the intercept of the In [(D2t -D20)/t] vs InT1 plot, R is
the gas constant and T is the absolute temperature. As a natural
logarithm transformation of Eq. (2) is commonly written as;
In


Dt 2 D0 2 =t InK 2 Q =RT

where Dt is the average grain size, D0 is the initial grain size and t
is the soaking time. It can be seen that Q obtained from the slope
(S) of the In [(D2t -D20)/t] vs InT1 plot, i.e. S = Q/R.
The activation energy of the TiMo alloys for grain growth
are listed in Table 3 by fitting the experimental data in Fig. 8.

Table 3 Activation energy of TiMo alloys for grain

growth.

Fig. 6 Linear relationship between lnD and ln t for the

grain growth of Ti4Mo and Ti20Mo alloys.

Alloy

Ti
2Mo

Ti
4Mo

Ti
15Mo

Ti
20Mo

Activation energy (kJ/mol)

65.30

83.30

220.52

272.16

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M A TE RI A L S CH A RACT ER IZ A TI O N 84 (2 0 1 3 ) 1 0 51 1 1

induces the drag effect, and the activation energy for grain
growth increases with extending the solution time.

3.3.

Fig. 8 Plots of In [(D2t -D20)/t] as a function of 1/T for solution

time at 60 min of TiMo alloys.

The activation energy increases with increasing Mo content. The

activation energy for grain growth of Ti4Mo alloy is 83.30 kJ/
mol, which is much lower than 272.16 kJ/mol for Ti20Mo alloy.
Many researches have been done to investigate the activation
energy for grain growth of titanium alloys. The differences in
activation energy for grain growth is found to be ascribed to
temperature or solute additions mainly [26,27]. The increase of
the temperature and the reduction of the solute addition promote the diffusion of atoms. Because of high solute content of
Ti20Mo alloy, the diffusion of Ti20Mo alloy across grain
boundary is more difficult than that of Ti4Mo alloy. Therefore,
Ti20Mo alloy needs higher activation energy for grain growth. A
number of studies [14,26,27] have been conducted to study the
effect of solution time on activation energy of titanium alloy and
the activation energy for grain growth of titanium alloy increased with extending the solution time. This increasing of the
activation energy can be explained by solute drag effect. At the
early stage of solution, the migration velocity of grain boundary
is faster than the diffusion of intracrystalline solute atoms, and
the solute atoms do not aggregate in the boundaries. As a result,
the grain boundaries are free from the solute drag effect and
have lower activation energy. The driving force of grain growth
decreases with the solution time extending, and then the
migration velocity of grain boundary decreased. So the amount
of solute atom which aggregated at boundaries increased with
decreasing the migration velocity of grain boundary [28].
Therefore, enrichment of solute atoms in the boundaries

Influence of Grain Size on the Mechanical Properties

Table 4 shows the variation of mechanical properties of the

alloys with the average -grain size. The room-temperature
strength and plasticity of TiMo alloys increase with the
increasing of Mo content and decreasing of grain size. It can be
obviously seen that the mechanical property of Ti20Mo alloy is
better than that of Ti4Mo alloy, the enhancement in mechanical property is mainly due to the refinement of grain size which
is caused by the addition of Mo. On the other hand, the strength
and plasticity for Ti20Mo alloy increase obviously with increasing the grain size, the same trend is also found in Ti4Mo
alloy. This phenomenon is mainly due to the Hall-Petch
mechanism and dislocation density variation, large increases
in the strength are ascribed to the decreasing of the grain size,
this is consistent with the research showing that both the
tensile and yield strength of B-modified Ti6Al4 V alloys
increased with decreasing the -grain size [29]. However, some
other strengthening methods also exist in the present alloys,
such as solution strengthening. But in Ti4Mo alloy, the grain
refinement effect for the improvement of mechanical properties
is not evidence, the crystal structure/phase and solution
strengthening may be the main reason. As a result, the increase
of Mo content in titanium alloy leads to grain refinement and
improvement of plasticity, both the room-temperature strength
and plasticity of TiMo alloys increase with increasing Mo
content and decreasing the -grain size.

4.

Conclusions

The microstructure and the grain growth kinetics of TiMo

binary alloys are studied and the following conclusions are
drawn from this work:
(1) Ti1Mo alloy mainly contains hexagonal phase, while
Ti4Mo alloy has some acicular grains precipitated in
grains. When Mo content increases to 10 wt% or
higher, the retained phase becomes the only phase.
(2) The grain growth kinetics of the alloys studied follows a
normal growth. The grain size of TiMo alloys increases
with the increasing of solution treatment time, and the
time exponent of Ti4Mo alloy (0.42) is higher than that of
Ti20Mo alloy (0.26) due to the low dislocation density.

Table 4 Mechanical properties of TiMo alloys.

Alloy

Ti4Mo

Ti20Mo

Solution
condition
900
900
900
900
800
800
800
800

C/1 h AC
C/2 h AC
C/4 h AC
C/6 h AC
C/1 h AC
C/2 h AC
C/4 h AC
C//6 h AC

Average
-grain size (mm)

Yield
strength
(MPa)

Ultimate tensile
strength (MPa)

Elongation
(%)

Area
reduction
(%)

0.0868
0.1405
0.1808
0.2163
0.0351
0.0525
0.0711
0.0845

628
620
617
614
871
866
860
848

799
787
784
786
898
893
890
877

18.5
17.0
16.5
15.5
21.5
20.0
18.5
19.5

58
55
49
52
74
76
73
73

M A TE RI A L S C HA RACT ER I ZA TI O N 84 ( 20 1 3 ) 1 0 51 1 1

(3) The grain growth rate of Ti4Mo alloy with temperature

is much faster than that of Ti20Mo alloy in the same
solution-treated time. Because of being free from the
solute drag effect, the activation energy for grain
growth of Ti4Mo alloy (83.30 kJ/mol) is also lower than
that of Ti20Mo alloy (272.16 kJ/mol).
(4) The room-temperature strength and plasticity of TiMo
alloys increase with the increasing of Mo content and
decreasing of grain size. It coincides with the Hall-Petch
mechanism.

Acknowledgements
This work is performed partially under the support of the
National Basic Research Development Program of China
(Grant Nos. 2007CB613805).

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