Scripta Materialia 138 (2017) 66–70

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Scripta Materialia

journal homepage: www.elsevier.com/locate/scriptamat

Regular Article

Mechanical properties of fully martensite microstructure in Ti-6Al-4V

alloy transformed from refined beta grains obtained by rapid heat
treatment (RHT)
Yan Chong a,⁎, Tilak Bhattacharjee a,b, Jangho Yi a, Akinobu Shibata a,b, Nobuhiro Tsuji a,b
a
Department of Materials Science and Engineering, Kyoto University, Kyoto, Japan
b
Element Strategy Initiative for Structural Materials (ESISM), Kyoto University, Kyoto, Japan

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

Article history: Fully martensite microstructures transformed from refined β grains were obtained in a Ti-6Al-4V alloy by rapid
Received 6 April 2017 heat treatment (RHT) into a single β phase region followed by water quenching. Ultrafine-grained equiaxed α +
Received in revised form 25 May 2017 β microstructure obtained by hot compression of martensite was used as the starting microstructure for subse-
Accepted 25 May 2017
quent RHT. By increasing the heating rate from 10 °C/s to 50 °C/s, the resulting β grain size was refined from 40 μm
to 8 μm, which was the smallest size of β reported so far. Both strength and ductility increased with decreasing the
Keywords:
β grain size, which was attributed to the reduced micro-crack lengths by fractography analysis.
Ti-6Al-4V © 2017 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.
Martensite
β grain size
Rapid heat treatment

Titanium alloys especially α + β titanium alloys have been widely
used in different industrial applications due to their unique combination
of attractive properties like high strength to weight ratio, exceptional
corrosion resistance as well as good biocompatibility [1]. Ti-6Al-4V is
the most widely used α + β titanium alloy which has been reported
to account for more than 50% of the worldwide titanium tonnage [1,
2]. Martensite microstructure of Ti-6Al-4V alloy obtained by solution
treatment in a single β phase region followed by water quenching is
comprised of fine α′-lamellae having various orientations (variants)
within coarse prior β grains. The grain size of β is usually hundreds of
microns or even several millimeters [3], because of rapid grain growth
in BCC structure of β phase. Compared with a lamellar microstructure
obtained by solution treatment and slow cooling, the martensite micro-
structure generally possesses higher strength but lower ductility.
Previous investigations [4–9] have shown that by using rapid heat
treatment (RHT) into the single β phase region (at a heating rate in
the order of tens or even hundreds degrees per second), a unique micro-
structure comprising relatively fine β-grains with fully transformed
intragranular α-lamellae can be obtained. This microstructure shows
much better balance of strength and ductility as well as good fatigue
performance, compared with coarse-grained counterparts [7]. Howev-
er, the smallest β-grain size obtained by the RHT method so far is still
30–50 μm because of the relatively coarse (~ 5 μm) equiaxed used as
the initial microstructure. The main purpose of the present study is to
⁎ Corresponding author.
E-mail address: chong.yan.6w@kyoto-u.ac.jp (Y. Chong).
explore the limit of β-grain size refinement that can be achieved via
RHT method by using UFG equiaxed α + β microstructure as the initial
microstructure. Mechanical properties of fully martensite microstruc-
tures transformed from the fine α + β grains are also discussed.
Chemical composition of the Ti-6Al-4V alloy used in the present
study was Ti-6.29Al-4.35V-0.155O-0.225Fe (in mass%). The β transus
temperature of this alloy was estimated to be ~970 °C. Cylindrical spec-
imens with 8 mm in diameter and 12 mm in height were cut from the
as-received billet and solution treated at 1050 °C for 1 h in vacuum
followed by water quenching to get fully martensite microstructure
shown in Fig. 1(a). The average α′-lamellae thickness in the martensite
microstructure was 1 μm. The specimens with the martensite micro-
structure were uniaxially hot compressed on a thermomechanical pro-
cessing simulator (Thermecmastor-Z) at the temperature of 700 °C
and strain rate of 0.01 s−1 to a true strain of 0.8. The specimens were
heated to the deformation temperature at a heating rate of 10 °C ∙s−1
and held for 20 min for homogenization before the hot compression.
In the thermomechanical processing simulator, the temperature of the
specimen was controlled by induction heating, so that rapid heating de-
scribed later could be also carried out. After the hot compression, the
samples were immediately reheated to a temperature in the single β
phase region (995 °C) at a heating rate of 10 °C ∙ s−1, 30 °C ∙ s−1 or 50
°C∙s−1 and held for 5 s before water quenching to room temperature.
After the thermomechanical process, the samples were cut in half
along a diameter of the cylindrical specimens. The sections parallel to
the compression axis and including the center of the samples were
then ground and polished in standard metallographical methods.

http://dx.doi.org/10.1016/j.scriptamat.2017.05.038
1359-6462/© 2017 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.
 Y. Chong et al. / Scripta Materialia 138 (2017) 66–70 67

Fig. 1. (a) Initial martensite microstructure transformed from coarse β grains. An EBSD IPF map. (b) IPF map of α phase before the hot deformation. The specimen for (b) and (c) was heated
to 700 °C at a heating rate of 10 °C∙s−1, held for 20 min, and then water-cooled without deformation. (c) IPF map of β phase before the hot deformation. (d) IPF map of α phase after the hot
deformation. (e) IPF map of β phase after the hot deformation. The colors in the IPF maps (b)–(e) indicate crystallographic orientation parallel to the compression direction, according to
the key stereographic triangles inserted.

Electrical polishing in a solution of 10% perchloric acid and 90% metha-
nol at −30 °C was conducted. Microstructural observations were car-
ried out at the center of the samples on the sections described above.
Electron backscattered diffraction (EBSD) investigations were conduct-
ed using TSL system attached to a field emission gun SEM (JEOL 7100F)
operated at an accelerating voltage of 15 kV. The collected data were an-
alyzed using OIM software. Micro-tensile specimens with a gauge
length of 2 mm, width of 1.2 mm and thickness of 0.5 mm were cut
from the center of the cylindrical specimens compressed. The tensile di-
rection was perpendicular to the compression axis. We have confirmed
in previous studies that the micro-tensile specimen could give reliable
stress-strain date equivalent to those obtained from standard-sized
specimen of the same material [10]. Tensile tests were conducted on
Shimadzu AG-X plus system at an initial strain rate of 8.3 × 10−4 s−1
at room temperature. The tensile strains of the micro-tensile specimens
were precisely measured by a digital image correlation (DIC) method.
Surfaces of the micro-tensile specimens were sprayed with white and
black contrast particles which acted as markers for the DIC analysis.
During the tensile test, the images of the micro-tensile specimens
were captured by a CCD camera at a speed of 10 frames per second.
After the tensile test, captured images were analyzed using Vic-2D com-
mercial software to determine the strain in the micro-tensile specimens
through tracking the positions of markers. For each condition, at least
two specimens were tested and the average values were used for eval-
uating strength and ductility.
The initial martensite microstructure shown in Fig. 1(a) had a large β
grain size which was measured to be ~ 200 μm by a line intersection
method on optical micrographs. Microstructure of the sample water
quenched before the hot compression was characterized. It is found in
the IPF maps (Fig. 1(b) and (c)) that during the holding period, the mar-
tensite microstructure was tempered and a small amount of β phase
formed, having the same orientation within the same prior β grain
(Fig. 1(b) and (c)). During the hot compression at relatively low tem-
perature (700 °C), the tempered α′-lamellae and a small amount of β
were supposed to change into equiaxed α grains via dynamic recrystal-
lization (probably via discontinuous dynamic recrystallization [11,12]),
which could be confirmed by various orientations of both α and β grains
shown in Fig.1 (d) and (e). Microstructure of the sample immediately
water quenched after the hot compression was characterized. Inverse
pole figure (IPF) maps indicating crystallographic orientation parallel
68 Y. Chong et al. / Scripta Materialia 138 (2017) 66–70

to the compression direction of the α and β phases are shown in

Fig. 1(d) and (e), respectively. An equiaxed microstructure with ultrafine
grain sizes (α grain ~ 500 nm, β grain ~ 200 nm) was obtained as expect-
ed. The volume fraction of retained β phase was about 4.0%. The β grains
with the ultrafine grain size would act as nuclei for α to β phase transfor-
mation in the subsequent rapid heat treatment.
The microstructures after RHT at different heating rates followed by
water quenching are shown in Fig. 2. Fully martensite microstructures
were obtained in all the specimens. The average grain sizes of prior β
were measured to be 40 μm, 15 μm and 8 μm for the heating rates of
10 °C∙s−1, 30 °C∙s−1 and 50 °C∙s−1, respectively. The β grain sizes ob-
tained by the RHT method were all much smaller than that of the initial
martensite microstructure. The β grain refinement was finer in the
specimens heat-treated at higher heating rate. The grain size of 8 μm ob-
tained in the specimen with the heating rate of 50 °C/s is the finest body
centered cubic (BCC) β grain size reported so far for Ti-6Al-4V alloy.
With the refinement of the β grain size, the average length of α′-lamel-
Fig. 3. Engineering stress-strain curves of the fully martensite microstructures with
lae formed within the β grain was significantly reduced. However, it
different β grain sizes (Dβ). Positions and values of the tensile strength and total
should also be noted that there existed a size gradient of β grains elongation are indicated for each curve.
along the radial direction of the cylindrical specimen possibly due to
higher temperature near the surface part in RHT by induction heating.
The distribution of the β grain size from the center to the surface in ductility increased with decreasing the β grain size. As the average β
the specimen is plotted for each heating rate condition in a supplemen- grain size decreased from 200 μm to 8 μm, the tensile strength increased
tary material (Fig. A). It was clearly shown that the β grain size was larg- from 1047 MPa to 1298 MPa while the total elongation also increased
er near the surface than that in the center regions. This phenomenon from 9.4% to 19.8%. This result suggested that by refining the β grain
indirectly affected the pinning effect for the grain growth of β grains size, the strength and ductility of fully martensite microstructures can
by remaining α grains during heating and holding processes, as α grains be simultaneously increased. The increase of strength was expected to
near the surface dissolved earlier. The area with uniform β grain sizes in be attributed to a grain refinement strengthening, since the α′-lamellae
the center decreased with the increase of the heating rate. width were reduced with the grain refinement of β. On the other hand,
In order to evaluate the effect of β grain size on mechanical proper- because the uniform elongation remained unchanged with the
ties of the fully martensite microstructures, micro-tensile specimens refinement of β grain size, as is indicated by the arrows in Fig. 3, the in-
were cut from the area with uniform β grain sizes and then tensile test- crease of total elongation was mostly attributed to the increase of post-
ed at room temperature. The engineering stress-strain curves of the uniform elongation.
specimens with different β grain sizes are shown in Fig. 3. All the curves In the previous studies [13], it is found that the martensite micro-
showed high yield strength but limited work-hardening followed by structure of Ti-6Al-4V alloy followed the quasi-cleavage fracture behav-
large post-uniform elongation, which was typical for martensite micro- ior. Therefore, the microstructures near the tensile fractured surfaces
structures of Ti-6Al-4V alloy [13]. Surprisingly, both strength and were observed in the specimens with different β grain sizes, with a

Fig. 2. EBSD IPF + IQ maps (a–c) indicating crystallographic orientations parallel to the compression direction as well as corresponding BSE images (d–f) of the fully martensite
microstructures after RHT and water quenching. (a) and (d) heating rate of 10 °C∙s−1; (b) and (e) 30 °C∙s−1; (c) and (f)50 °C∙s−1.
 Y. Chong et al. / Scripta Materialia 138 (2017) 66–70
special attention to the size and distribution of micro-cracks. The EBSD
image quality (IQ) maps of specimens with the largest and smallest β
grain sizes, together with the plot showing the evolution of average
crack length with β grain size are shown in Fig. 4, in which the micro-
cracks are indicated as dark regions. Regardless of the β grain size,
micro-cracks were found to form, and the cracks propagated along α′-
lamellae. In order to statistically measure the average length of the
micro-cracks, at least five areas like Fig.4 were observed for each speci-
men. The average crack lengths in the specimens with mean β grain size
of 200 μm, 40 μm, 15 μm, and 8 μm were 80 μm, 30 μm, 20 μm, and 10
μm, respectively. It was quite clear that with the refinement of β grain
size, the average micro-crack length decreased. This was due to the
fact that the propagation of micro-cracks along one α′-lamellae got
blocked when meeting another α′-lamellae with different orientations.
Therefore, in the specimen with smaller α′-lamellae length, the chance
of micro-cracks getting blocked significantly increased and subsequent-
ly the average crack propagation length was reduced, which was
believed to be the main reason for the increased post-uniform elonga-
tion with the refinement of the β grain size.
To summarize, rapid heat treatments to a temperature in the single β
phase region followed by water quenching were carried out on the UFG
equiaxed microstructure of Ti-6Al-4V alloy formed by hot-deformation.
Full martensite microstructures with prior β grain sizes as small as 8 μm
Fig. 4. EBSD IQ maps near fracture surfaces of the tensile fractured specimens with the average β grain sizes (Dβ) of 200 μm (a) and 8 μm (b). (c) The plot of average crack length against the
averageβ grain size with error bas include.
69
could be obtained when the heating rate was 50 °C∙s−1, which was the
smallest β grain size reported by now. With the refinement of the β
grain size, both strength and ductility of the final martensite specimens
increased. The tensile strength and total elongation of the sample with
the minimum β grain size of 8 μm reached 1298 MPa and 19.8%. The
total elongation was twice of that with a coarse β grain size (200 μm).
The improvement in total elongation was attributed to the reduced
micro-crack length associated with the decrease in the length of α′-la-
mellae. The present result would open a possibility for obtaining the
full martensite microstructures transformed from fine β grain sizes in
Ti-6Al-4V alloy, which process higher strength and ductility comparable
to the bimodal microstructures of the alloy. Superior creep resistance
nature of the martensite microstructures could be expected at the
same time.
Supplementary data to this article can be found online at http://dx.
doi.org/10.1016/j.scriptamat.2017.05.038.
Acknowledgement
The authors were financially supported by the Cross-Ministerial
Strategic Innovation Promotion Program on Structural Materials for In-
novation (SIP-SMI), and the Elements Strategy Initiative for Structural
Materials (ESISM). The supports are gratefully appreciated.
70 Y. Chong et al. / Scripta Materialia 138 (2017) 66–70

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