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Effects of Temporary Alloying and Severe Plastic Deformation on

Microstructure Evolution and Mechanical Properties of Ti-Alloys: A
Comparative Study

Article  in  Transactions of the Indian Institute of Metals · February 2019

DOI: 10.1007/s12666-019-01594-3

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Effects of Temporary Alloying and Severe
Plastic Deformation on Microstructure
Evolution and Mechanical Properties of Ti-
Alloys: A Comparative Study

S. M. Jagadeesh Babu, S. V. S. Narayana

Murty, N. Prabhu, R. Kapoor,
R. N. Singh & B. P. Kashyap

Transactions of the Indian Institute of

Metals

ISSN 0972-2815

Trans Indian Inst Met

DOI 10.1007/s12666-019-01594-3

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Trans Indian Inst Met
https://doi.org/10.1007/s12666-019-01594-3

TECHNICAL PAPER

Effects of Temporary Alloying and Severe Plastic Deformation

on Microstructure Evolution and Mechanical Properties of Ti-
Alloys: A Comparative Study
S. M. Jagadeesh Babu1 • S. V. S. Narayana Murty2 • N. Prabhu3 •

R. Kapoor4 • R. N. Singh4 • B. P. Kashyap5

Received: 1 September 2018 / Accepted: 17 January 2019

Ó The Indian Institute of Metals - IIM 2019

Abstract Near-a (VT 20) and a ? b (Ti–6Al–4V) Ti morphology for THP alloy, whereas it was equiaxed for as-
alloys having similar initial grain morphology with received VT 20 and CR 750 alloy. An additional attempt
equiaxed a in transformed b were subjected to was made on the CR alloy towards determining the mag-
microstructure refinement processes by thermohydrogen nitudes of strain rate sensitivity index (m) through differ-
processing (THP) and caliber rolling (CR), respectively. ential strain rate test conducted over a number of strain rate
The microstructure analysis after THP and CR of the alloys change cycles at 850 °C and 927 °C. Both THP and CR
revealed the change in morphology and refinement of processes resulted in grain refinement and the change in
microstructure. The microstructure analysis after initial morphology of microstructure.
constant strain rate tests at 850 °C exhibited needle-like
Keywords Thermohydrogen processing
Caliber rolling

VT20
Ti–6Al–4V
Grain refinement
& S. M. Jagadeesh Babu
babu.iitb2013@gmail.com
S. V. S. Narayana Murty 1 Introduction
susarla.murty@gmail.com
N. Prabhu Near-alpha titanium alloy, an ideal material for aeroengine,
nprabhu@iitb.ac.in can be used in operating temperature of about 600 °C. It
R. Kapoor exhibits superior mechanical properties at elevated tem-
rkapoor@barc.gov.in perature, especially creep resistance [1]. The Ti–6Al–4V is
R. N. Singh a two-phase a ? b alloy, a workhorse alloy prominently
rnsingh@barc.gov.in used for aerospace applications [2], due to exceptional
B. P. Kashyap high-temperature properties and formability [3]. The
bpk@iitj.ac.in lamellar microstructure can be broken to produce equiaxed
1
or bimodal microstructure by thermomechanical process-
School of Mechanical Engineering, REVA University,
Bengaluru 560064, India
ing, which helps to balance the properties [2]. Studies have
2
reported grain refinement through various ways: addition of
Special Materials Division, Vikram Sarabhai Space Center,
ISRO, Trivandrum 695022, India
boron [4], alloying with hydrogen [5] and severe plastic
3
deformation (SPD) [3, 6] in titanium-based alloys. Ther-
Department of Metallurgical Engineering and Materials
Science, Indian Institute of Technology Bombay, Mumbai
mohydrogen processing (THP) uses hydrogen as temporary
400076, India alloying element to refine the microstructure through
4 modifying the phase compositions, forming
Mechanical Metallurgy Division, Bhabha Atomic Research
Centre, Anushaktinagar, Mumbai 400085, India metastable phases, phase transformation, etc. This results
5 in improved mechanical properties in titanium alloys [5, 7].
Department of Metallurgical and Materials Engineering,
Indian Institute of Technology Jodhpur, Karwar 342037, Unlike conventional microstructural refinement techniques,
India THP does not require mechanical working to refine the

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microstructure [5]. Also, it has been established that the
grain size of metals and alloys can be significantly refined
to ultrafine (\ 1 lm) or even to the nanometer (\ 100 nm)
range through SPD process [7]. Development of novel
processes to impart ultrafine microstructure has great
interest in the superplastic behavior of metallic materials at
low temperatures and/or high strain rates [6]. Microstruc-
ture refinement significantly decreases superplastic tem-
perature, thereby leading to a decrease in processing tool
costs and material savings due to reduced contamination
[8]. The present article is an attempt to study the com-
parative effects of temporary alloying (hydrogenation) and
SPD (caliber rolling) processes on the microstructure and
mechanical behavior of near-a VT 20 and a ? b Ti–6Al–
4V alloy.
2 Experimental Work
The VT 20 alloy was procured from Hindustan Aeronau-
tical Limited (HAL), Nasik, India. The nominal composi-
tion of VT 20 alloy is given in Table 1. The alloy was
prepared by removing oxide layer or dirt from the surface
before subjecting to hydrogenation process. From the as-
received VT 20 alloy, pieces of 42 mm 9 13 mm 9 12
mm were cut and then all the surfaces were polished on
emery papers of 220, 500 and 800 grit. The polished
sample was cleaned in acetone and placed in a modified
Sievert’s apparatus, which was evacuated to a vacuum of
10-4 Torr. The sample was heated to 750 °C, and the
desired amount of high-purity hydrogen gas was released
into the apparatus. The samples were hydrogenated to
0.18 wt% H and 0.4 wt% H levels at a temperature of
750 °C and subsequently air-cooled to room temperature.
Ti–6Al–4V alloy was cut into blocks of
45 9 45 9 200 mm3 sizes from the initial bar and then
processed by caliber rolling (CR) at temperatures of
750 °C and 850 °C at Indian Space Research Organisation
(ISRO), Trivandrum, India. The nominal composition of
Ti–6Al–4V alloy is given in Table 2. The caliber rolling
was carried out through a series of roll passes in a rolling
mill with grooved rolls and with intermittent heating. The
input material blocks were heated in an electric billet
heating furnace with a temperature accuracy of 75 °C. The
reduction direction was changed in increments of 90° by
rotating the material one quarter turn in each pass.
Table 1 Chemical composition of VT 20 (near-a titanium alloy)
Element Al Zr C Fe Si
wt% 5.9 ± 0.4 2.1 ± 0.2 0.1 0.3 0.15
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Trans Indian Inst Met
Immediately after final pass, the rolled rods were water-
quenched. Caliber rolling at two different temperatures of
750 °C and 850 °C was done for final reduction to
12 9 12 9 L mm3 (where L = Length of the rods),
imposing a cumulative reduction of * 92% and a cumu-
lative strain of 2.6. Based on the caliber rolling tempera-
tures employed, these rolled rods were designated as CR
750 and CR 850, respectively.
The VT 20 and caliber-rolled Ti–6Al–4V alloys were
subjected to tensile deformation at the temperature of
850 °C and a strain rate of 1 9 10-3 s-1. A differential
strain rate test up to failure of the sample was conducted on
CR 750 material over a number of strain rate change cycles
at 850 °C and 927 °C to determine strain rate sensitivity
index (m). High-temperature lubricants such as glass
coating and delta glaze were used to avoid the adverse
effects of oxidation. Microstructure examination was car-
ried out on VT 20 and Ti–6Al–4V alloys, for which the
samples were prepared by standard metallographic tech-
nique and using Kroll’s reagent as an etchant.
3 Results and Discussion
3.1 Initial and Post-processed Microstructures
of Near-a and a 1 b Ti Alloys
The initial microstructures of both VT 20 and Ti–6Al–4V
alloys are shown in Fig. 1a, b. These microstructures
comprise of mat-like interweaving elongated grains of a
(white) and b (dark) phases (Fig. 1a) and equiaxed a with
transformed b structure (Fig. 1b), respectively. The
microstructures after hydrogenation to 0.18 wt% H and
0.4 wt% H are shown in Fig. 1a1, a2. The mean grain size
of VT20 Ti alloy in as-received condition has been deter-
mined to be 5.4 ± 0.5 lm. Upon hydrogenation to
0.18 wt% H and 0.4 wt% H, the microstructure exhibits
elongated grains with the mean grain sizes of
3.1 ± 0.2 lm and 2.8 ± 0.2 lm, respectively. Kohn and
Ducheyne [9] reported that the addition of hydrogen has
resulted in small a-grain sizes, reduced aspect ratios and
the disappearance of continuity of the a-phase at the prior
b-grain boundaries. Studies in [10, 11] have described the
hydrogenation and dehydrogenation processes leading to
an ultrafine grain structure. The migration of alloying
elements (Ti, Al and V) in the presence of hydrogen leads
O N H Mo V Ti
0.15 0.05 0.0015 1.4 ± 0.1 1.6 ± 0.1 Bal
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Trans Indian Inst Met
Table 2 Chemical composition of Ti–6Al–4V (a ? b titanium) alloy
Element Al V Fe
wt% 6.19 4.05 0.03
Fig. 1 Initial microstructure and its evolution in VT 20 alloy and Ti–6Al–4V alloy before; a hydrogenation b caliber rolling; after hydrogenation
(a1, a2) and caliber rolling at 750 °C (b1), 850 °C (b2)
to the formation of lamellar structure and is stable below
the b-transus temperature for Ti–6Al–4V alloy [12]. The
changes in the specific volume of the phases determine the
morphology of the structure (equiaxed or elongated) [5].
The transformation of a phase into aH and bH, as over-
saturated by the addition of hydrogen, leads to the breakup
of a phase [13]. The hydrogenation causes the eutectoid
reaction; a ? bH? aH leading to near equiaxed fine aH-
? bH microstructure followed by decomposition reaction
bH ? a ? d and aH ? a ? d.
Similarly, microstructures after caliber rolling process at
temperatures of 750 °C (CR 750) and 850 °C (CR 850) are
shown in Fig. 1b1 and b2, respectively. Prior to caliber
rolling, Ti–6Al–4V alloy microstructure is comprised of
equiaxed morphology with mean grain size of a phase
being 15 lm. Upon caliber rolling, equiaxed structure
changes into lamellar elongated grains with the mean grain
sizes of 0.53 lm and 1.05 lm for caliber-rolled tempera-
tures 750 °C and 850 °C, respectively [14]. Murty et al.
[15] have shown that upon multipass caliber rolling, the
Widmanstatten colonies (a ? transform b) transform to a
lamellar structure with complete fragmentation of the b-
phase and its distribution in the a-phase matrix.
C O N H Ti
0.0171 0.112 0.0031 0.004 Bal
3.2 Microstructure Evolution and Flow Behavior
of THP and CR Alloys
Figure 2 shows stress–strain curves and microstructures
after tensile deformation at the temperature of 850 °C for
near-a VT20 alloy and Ti–6Al–4V alloy. Stress–strain
curves are shown from the onset of plastic strain, and they
exhibit continuous softening in all the cases (Fig. 2a).
Interestingly, irrespective of the process, the stress–strain
behavior of as-received VT 20 and caliber-rolled Ti–6Al–
4V alloy show similar trend with the increase in strain. But,
after reaching the strain level of 1.0, the stress–strain
behavior of Ti–6Al–4V alloy deviates to give more elon-
gation as compared to that of VT 20 alloy. As described by
Zong et al. [16], the high-temperature deformation mech-
anisms of titanium alloys can be explained by the shape of
stress–strain curves. The continuous flow softening can be
attributed to morphological change from lamellar to
equiaxed (globularization), dynamic recrystallization
(DRX) or adiabatic heating [16]. The microstructures show
basket weave (better work hardening behavior and
strength), globular lamellar (better ductility) and equiaxed
(best ductility) morphology [17]. VT 20 alloy shows fine
equiaxed, needle-like microstructure (Fig. 2b, c), whereas
Ti–6Al–4V alloy shows an equiaxed microstructure
(Fig. 2d). However, Zong et al. [16] have shown equiaxed
a phase and transformed b microstructure for the
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Trans Indian Inst Met

Fig. 2 a Stress–strain curves; micrographs of b as-received c 0.4 wt% H (with magnified inset) of VT 20 alloy and d CR 750 Ti–6Al–4V alloy
after tensile deformation to failure at the temperature of 850 °C and strain rate of 1 9 10-3 s-1

unhydrogenated alloy and hydrogenated (0.1 wt%) alloy,
indicating deformation in the a ? b phase region. Further,
for the hydrogen content of 0.2 wt%, the microstructures
are comprised of needle-like structure (martensite), indi-
cating that the deformation has occurred in single-phase b
region [16]. The microstructures reported by Zong et al.
[16] in the a ? b and b phase region are consistent with the
present study as shown in Fig. 2 b, c. Park et al. [18]
investigated microstructural mechanisms (globularization)
of a Ti–6Al–4V alloy at deformation temperature of
800 °C and over the strain rate range of 10-3 s-1 to 1 s-1.
Microstructural evolution during dynamic globularization
has been examined, which are associated with kinking and
fragmentation of lamellar plates [18].
It is found that, at 850 °C, the sample of caliber-rolled
Ti–6Al–4V alloy could be deformed through more number
of cycles as compared to that at 927 °C (Fig. 3a). This can
be attributed to oxidation and grain growth effects at the
higher test temperature. The microstructures show fine
equiaxed structure at the deformation temperature of
850 °C (Fig. 3b) and bimodal distribution at the deforma-
tion temperature of 927 °C (Fig. 3c). A study by Kashyap
and Mukherjee [19] on the superplastic behavior of a
microduplex stainless steel shows the occurrence of grain
growth and breaking up of elongated grains concurrent to
deformation. Microstructural instabilities lead to strain
hardening or strain softening causing nonuniqueness in the
flow behavior [19]. They have concluded that, at lower
temperature of 810 °C, strain softening is dominant owing
to the evolution of elongated grains toward equiaxed shape
[19]. The strain rate sensitivity index (m) obtained for cycle
I shows two slope behaviors at both the temperatures
850 °C and 927 °C. The m values have been found to range
from 0.23–0.34 to 0.03–0.34 depending on strain rate range

Fig. 3 a Stress–strain plot of CR 750 Ti–6Al–4V material from strain rate jump test at the test temperatures of 850 °C and 927 °C;
microstructures (along with the enlarged views of encircled parts) after the failure of the specimens at the test temperatures b 850 °C c 927 °C

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Trans Indian Inst Met
at the test temperatures of 850 °C and 927 °C, respectively.
A continuous increase in m with strain can be attributed to
change of elongated grains into equiaxed grains and also
the flow softening [20].
4 Conclusions
Although the two alloys belonged to two distinct alloy
systems (near-a and a ? b), they were both subjected to
methods aimed at refining their microstructure and
enhancing their mechanical behavior. The mean grain size
of VT 20 alloy upon hydrogen charging to 0.18 wt% H and
0.4 wt% H get refined from 5.4 ± 0.5 lm to 3.1 ± 0.2 lm
and 2.8 ± 0.2 lm, respectively. Similarly, caliber rolling
of Ti–6Al–4V alloy resulted in change of equiaxed mor-
phology with mean grains size of 15 lm to lamellar
elongated grains with a mean grain size of 0.53 lm and
1.05 lm for caliber-rolled temperatures of 750 °C and
850 °C, respectively. While the VT 20 material was tem-
porarily alloyed with hydrogen, the Ti–6Al–4V alloy was
subjected to severe plastic deformation through caliber
rolling. Both THP and CR processes were noted to assist in
grain refinement and the change in morphology of
microstructure. However, it seemed that the nature and
extent of grain refinement and morphological changes in
THP and CR samples were little different. The initial
constant strain rate test at 850 °C exhibited flow softening
in stress–strain behavior and also showed microstructures
with equiaxed and needle-like morphologies. These mor-
phologies thus indicated the equiaxed and needle-like
structures to be the consequence of deformation in the
(a ? b) and b phase regimes, respectively. It was found
that, at 850 °C, the sample could be deformed through
more number of strain rate change cycles as compared to
that at 927 °C, which could be attributed to the effect of
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oxidation and grain growth under the latter condition of
higher temperature.
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