Journal of Alloys and Compounds 695 (2017) 3495e3502

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Journal of Alloys and Compounds

journal homepage: http://www.elsevier.com/locate/jalcom

High strength in high Nb containing TiAl alloy sheet with fine duplex
microstructure produced by hot pack rolling
Haitao Zhou, Fantao Kong*, Xiaopeng Wang, Yuyong Chen
National Key Laboratory for Precision Hot Processing of Metals, School of Materials Science and Engineering, Harbin Institute of Technology, Harbin, 150001,
PR China

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

Article history: The Ti-44Al-8Nb-(W, B, Y) alloy sheet with a large thickness reduction of 85% was successfully obtained
Received 3 August 2016 by hot pack rolling with 25% reduction per pass. The original coarse nearly lamellar structure with mean
Received in revised form grain sizes of 120 mm was converted into a fine duplex microstructure with mean grain sizes of 5.3 mm.
16 November 2016
The as-worked alloy contains more than 70% vol. % of disordered a phases before the hot pack rolling.
Accepted 1 December 2016
Available online 2 December 2016
After the repeated deformation, these disordered a laths transform into interrupted fine recrystallization
and recovery sub-grains. Then both a / a2 ordering transformation and g laths precipitation from the
interrupted a phases take place during the cooling. Furthermore, the g grains and g laths also carry large
Keywords:
High Nb containing TiAl alloy sheet
strains and produce a large number of dislocations. These dislocations tangle and form dislocations
Hot pack rolling networks which promote the discontinuous dynamic recrystallization nucleation and growth. As
Recovery deformation proceeds during the subsequent hot pack rolling, the recrystallization, recovery and phase
Recrystallization transformations of the previously formed recrystallization and recovery regions take place at tri-
Disordered a phases boundaries and inside the lamellar, resulting in the formation of fine duplex microstructure. At room
temperature, the as-rolled alloy exhibits yield strength, ultimate tensile strength and ductility of
962 MPa, 1174 MPa and 1.01%, respectively. When temperature becomes as high as 850
C, the failure
strength still remains higher than 630 MPa with a good elongation value of above 45%.
© 2016 Published by Elsevier B.V.

1. Introduction well-fabricated TiAl alloy sheets at present still have drawbacks,

Due to the good mechanical properties at elevated tempera-
tures, the high Nb containing TiAl alloy [1e5] sheets are thought to
further expand the aerospace applications such as inlet flaps,
nozzle tiles for gas turbine engines, back structures for scramjets
and thermal protection shields [6,7] to higher temperature. Yet, it is
still a huge challenge to produce high Nb containing TiAl alloy
sheets because of the narrow hot processing windows and large
tensile stress in the surface [4,8]. Another restricting factor for the
application of high Nb containing TiAl alloys is the poor room-
temperature ductility. Hot pack rolling, as the most effective way
to fabricate TiAl alloy sheets, is an attractive and highly efficient
means to obtain product forms with good mechanical properties
[4,9]. However, there are still obstacles in acquiring fine micro-
structures and excellent surface quality without cracks simulta-
neously, by increasing reduction per pass [8,10]. Furthermore, the
* Corresponding author.
E-mail address: kft@hit.edu.cn (F. Kong).
including insufficient tensile strength at ambient temperature,
remnant lamellar colonies and coarse microstructures. It seems
that the ultimate tensile strength (UTS) of less than 900 MPa at
room temperature and 720 MPa at 800
C of as-rolled alloys could
not meet the expectations for high Nb containing TiAl alloys as
structural materials [4,8,11]. Moreover, the coarse microstructures
and remnant lamellar structures are harmful to the mechanical
properties [12,13].
In terms of the hot pack rolling, the high Nb containing alloy
billets are often annealed within (aþg)-phase field for hours [4].
The disordered high-temperature b phase can be induced by adding
moderate b stabilizers W and Nb, which serve as a lubricant during
thermo-mechanical processing. The b0 content depends on the
content of Al and Nb. It is deduced that the critical value for the
occurrence of b0 is over 8Nb when the Al content is 44 at% from the
phase equilibria in Ti-Al-xNb ternary systems [14]. Also, there are
almost no b0 phase in the as-cast and as-forged Ti-44Al-8Nb-(W, B,
Y) alloy [15,16] at room temperature and 1250
C. Therefore, more
attention is paid to the disordered a phases and g phases in this

http://dx.doi.org/10.1016/j.jallcom.2016.12.005
0925-8388/© 2016 Published by Elsevier B.V.
3496 H. Zhou et al. / Journal of Alloys and Compounds 695 (2017) 3495e3502
research. Deformation and phase transformation of these a and g
grains will occur repeatedly during hot pack rolling. However, over
the past decades, research on the recovery and recrystallization of
disordered a and g phases during hot pack rolling about TiAl alloys,
especially for high Nb containing TiAl alloys is inadequate. The role
of the disordered a phases at the deformation temperature is also
frequently ignored. In this study, the high performance of Ti-44Al-
8Nb-(W, B, Y) alloy sheet has been successfully achieved via an IM
route by hot pack rolling. The focus is on the formation mechanism
of fine and homogenous duplex microstructures, especially for the
role of recovery and recrystallization of the disorderd a laths and g
laths in lamellar evolution.
2. Experimental
A plate billet with a size of 70  65  20 mm3 was cut from the
as-forged pancake, and encapsulated in a stainless steel can. The
billet with pack was rolled on a mill with a roller dimension of
Ф350 mm  400 mm. Preheating for about 2 h and reheating be-
tween two passes for about 15 min at a temperature of 1250
C in
the (aþg) phase region were carried out on the packed billet, which
was rolled for six passes with a total thickness reduction of 85%. The
crack-free sheet is shown in Fig. 1. The nominal rolling speed was
smaller than 0.2 m/s. The as-rolled sheet was annealed at 900
C for
6 h and furnace-cooled to room temperature. In order to preserve
the microstructure before hot rolling for subsequent microstruc-
tural characterization, the specimens were water quenched
immediately after the heat treatment at 1250
C for 2 h. The mi-
crostructures were characterized by scanning electron microscopy
(SEM) in the backscattered electron mode (BSE), electron back-
scattered diffraction (EBSD) and transmission electron microscope
(TEM) techniques. Flat tensile test specimens with a gauge section
of 18  5  2 mm3 for room temperature and high temperature
were cut from the as-rolled alloy sheet along the rolling direction
(RD) and conducted with a strain rate of 2  104 s1 and 5  104
s1, respectively.
3. Results and discussion
Fig. 2(a) shows the microstructure of the as-forged alloy, which
has a nearly lamellar microstructure composed of plentiful lamellar
colonies with mean colony sizes of 120 mm, and a small amount of
10 mm fine equiaxed g grains along its boundaries. These lamellar
colonies feature a coarsened and bent lamellar structure. In this and
subsequent BSE micrographs, the dark, grey and white parts are g,
a2 and b0 phase, respectively. The microstructure after 2 h
annealing at 1250
C, followed by water quenching is shown in
Fig. 2(b). The g phases exist in the form of fine particles with
equiaxed and laths morphology. Yet, the ordered a2 phases
constitute the major and continuous phase with 70% vol. %, and will
transform into disordered a phases within (aþg) phase region.
Therefore, the as-worked TiAl alloy has more than 70% vol. %
Fig. 1. Appearance of Ti-44Al-8Nb-(W, B, Y) alloy sheet with a total reduction of 85%.
disordered a phases prior to the hot pack rolling. The disordered a
phases are softer and easier to deform, compared to ordered a2 and
g phases. Evidence also can be found in the hot compression ex-
periments of high Nb containing TiAl alloy [16].
The microstructure of the as-rolled Ti-44Al-8Nb-(W, B, Y) alloy
is illustrated in Fig. 3. The as-rolled alloy microstructure mainly
consists of fine and homogeneous duplex (DP) microstructures
with little remnant lamellar (RL). The microstructure details of the
RL and DP regions are magnified in Fig. 3(b) and (c). The grains in RL
structures are elongated and coarsened with interfaces, mostly
parallel to the rolling direction. The DP area is a duplex micro-
structure with mean grain sizes of 5.3 mm. It is smaller than the
10 mm of the Ti-45Al-7Nb-0.3W alloy [8] and 15 mm of the Ti-45Al-
8.5Nb-(W, B, Y) alloy [4], and even close to the 5 mm of the Ti-46Al-
9Nb alloy by PM [11]. The refinement of the microstructure is
mainly due to the large 25% reduction per pass and 85% total
thickenss reduction. The fine a2/g lamellar colonies with random
orientations (marked with red lines) are transformed from the
interrupted a grains generated through the recovery and recrys-
tallization of a laths. Additionally, the finer duplex area is found in
the white rectangle in Fig. 3(c), which may be caused by a large
deformation strain. Recrystallization is more likely to take place in
such regions with coarsening and bending laths marked in Fig. 3(c)
if the deformation is continued. As the addition of Nb element can
reduce the stacking fault energy in a high Nb containing TiAl alloy
[17] and further promote the movements of partial dislocations,
leading to the formation of twins. Some twins are found (marked
with a green line) in the as-rolled alloy.
Generally, it is complex for the conversion of the disordered a
laths and g laths into the duplex microstructure during hot pack
rolling. Shen reported that the interruption, rotation, bending,
kinking, and breaking down of lamellar colonies were responsible
for microstructure evolution of the Ti-45Al-8.5Nb-(W, B, Y) alloy
[4]. Yet, the specific ‘breaking down’ of lamellar colonies was not
pointed out. The exact mechanism for lamellar conversion can be
clarified by EBSD images in the RL region, as shown in Fig. 4. Parts of
the disordered a laths are broken into interrupted a grains such as
C, D and E with the same orientation, marked in Fig. 4(a and b),
implying that these grains come from a unique lath. Yet, some new
a grains B and F are formed in a subsequent process, exhibiting the
different orientation from the original lath. The other part of a laths
forms a2/g lamellae, marked by arrows in Fig. 4(c).
Additionally, the coarsened g laths are broken into fine g grains,
exhibiting a slight elongation along the rolling direction, as shown
in Fig. 4(d). The recrystallization and recovery regions, either at tri-
boundaries or inside lamellar, will continue to deform into finer
microstructures by a repeated large reduction per pass. Fig. 4(a)
shows that the direction of the white and black lines represents two
different lamellar colonies. The white ellipse ring located at the
boundaries of these lamellar colonies, and the black one inside the
lamellar, contain a relatively high amount of finer grains and sub-
structures, implying the occurrence of recovery and
 H. Zhou et al. / Journal of Alloys and Compounds 695 (2017) 3495e3502 3497

Fig. 2. Microstructures of (a) the as-forged alloy, (b) the as-quenched alloy after 2 h annealing at 1250
C.

Fig. 3. SEM-BSE of (a) as-rolled Ti-44Al-8Nb-(W, B, Y) alloy and magnification of (b) RL and (c) DP region. The rolling direction is shown in the insets.

recrystallization. The fact that the DRX takes place at triangle
lamellar boundaries, followed in lamellar colonies, can also be
found in Ref. [18].
The conversion mechanism of g laths into g grains or sub-grains
can be explained as follows. Fig. 4(e and f) shows the magnification
of the area outlined in white in Fig. 4(c). The analyzed g grains and
its corresponding pole figures (PFs) are serially numbered from 1 to
8. From the PFs in Fig. 4(g), the large misorientation among g grains
1e4, and 6 indicates that the g parent laths deform during the
repeated rolling process and form different orientation g grains.
The misorientation between 2 and 5 as well as 2 and 7 are 0.8
and
2.9
, respectively, indicating the same orientation of these sub-
grains. These sub-grains may transform into new grains during
the subsequent deformation. Additionally, some new g grains are
3498 H. Zhou et al. / Journal of Alloys and Compounds 695 (2017) 3495e3502

Fig. 4. EBSD images of the as-rolled Ti-44Al-8Nb-(W, B, Y) alloy (aed) overall microstructure of RL region: (e, f) magnification of white region in (a), (a, c, e) phase distribution, (b)
inverse pole figure, (d, f) unique grain color figure. (g) The PFs (1e8) corresponding to the numbered grains or sub-grains in (f).

found in these elongated coarsened g laths with different colors
from the matrix, such as grains 6 and 8. These finer new grains can
be suggestive of discontinuous dynamic recrystallization (DDRX).
DDRX is known to require a minimum amount of plastic defor-
mation and incubation time [19].
The irregular shaped a grains with different orientations in
Fig. 5(a) are formed by the mechanisms of DRV and DRX at 1250
C.
It has also been confirmed that the a/a2-phase tends to DRX for the
TNM alloy by isothermal compression at 1220
C [20]. The wavy
occurrence of a2-grains is a typical feature of DRX. On one hand,
some a phases will directly transform into a2 phases during the
cooling. On the other hand, the g laths will precipitate from the a
grains when the alloy cools to Te, as the multi-pass hot pack rolling.
Fig. 3(c) also confirms that the as-rolled microstructure consists of
g grains and a2/g lamellar colonies. Yet, the newly formed finer g
laths in a grains may not be detected as the scanning interval of
0.25 mm is larger than the thickness of newly formed g laths by
EBSD measurement.
The g grains or sub-grains at the boundaries or inside the
lamellar will continue to deform and form a finer microstructure by
 H. Zhou et al. / Journal of Alloys and Compounds 695 (2017) 3495e3502
Fig. 5. EBSD images of the as-rolled Ti-44Al-8Nb-(W, B, Y) alloy (a, b) phase distribution of DP region: (a) a2 phases, (b) g phases, (c), (d) the magnification of the area 2 and 3 in (b).
repeated large rolling reduction per pass. Two kinds of DDRX g
grains are found in regions 1 and 2 in Fig. 5(b). When the driving
force generated by deformation is greater than the recrystallization
activation energy, the recrystallization occurs by nucleation and
growth, such as the g grains in region 1. When the driving force is
not enough, the fine equiaxed g phases grains will form in the
interior of the g grains, and the growth tendency is small, just as the
grains in region 2. The difference between the g grains in regions 1
and 2 may be induced by the deformation imposed on each g grain.
The g grains in region 3 contain many low angle boundaries,
namely LAGS (blue in Fig. 5(d)). The misorientation of these g sub-
grains is 0.8
e2.8
, indicating that the sub-grains are formed by
recovery. LAGBs are the features of substructures formed during
deformation with the volume of 24.3%. The substructures (recovery
region) can be the nuclei for recrystallization and grow during the
subsequent rolling pass. So both recrystallization and recovery play
important roles in forming g grains.
Fig. 6 shows the images of the as-rolled alloy obtained by TEM
and the selected area diffraction patterns (SADPs) of corresponding
phases. Fig. 6(a) is the remnant lamellar composed of a black a2
phase interspersed with many white g laths with high densities of
dislocations, showing that the coarsening of g lath is implemented
by a lath decomposition. This phenomenon was also found in the
pack rolled Ti-44Al-6V-3Nb-0.3Y alloy [21]. The coarsened g laths
carry the major part of the strain and produce a large number of
3499
dislocations. These dislocations tangle and form dislocations net-
works, which promote the DDRX nucleation and growth. As
deformation proceeds, the coarsened g laths with high density
dislocations are broken down into fine recrystallized g grains.
Newly recrystallized g grains are formed through the rearrange-
ment of sub-structure. Dislocations and substructures also can be
seen in g phases, as seen in Fig. 6(bed).
The fine recrystallized g grains without dislocations distributed
within the lamellar colony are found in Fig. 6(c). In fact, recrystal-
lization g grains can be easily activated due to the high density
dislocations and interfacial strain energy induced by hot defor-
mation. Fig. 6(e) shows that the g grains consist of recovered sub-
grains containing high densities of dislocations and substructures
as well as a few fine equiaxed grains free of dislocations (in white).
These finer recovered sub-grains were easily consumed by the
recrystallized grains due to their higher stored energies [13]. Of
course, there is such a region that consists of recrystallized g grains
almost free of dislocations due to the sufficient driving force
generated from the deformation for dynamic recrystallization. By
the repeated recrystallization and recovery of a and g phases and
phase transformation of a phases, the final as-rolled alloy consists
of recrystallized g grains, almost free of dislocations and a2 grains,
as seen in Fig. 6(f).
The tensile strength-strain curves for specimens prepared along
the rolling direction and tested at room temperature and high
3500 H. Zhou et al. / Journal of Alloys and Compounds 695 (2017) 3495e3502

Fig. 6. TEM images of the as-rolled Ti-44Al-8Nb-(W, B, Y) alloy: (a) remnant lamellar, (b) dislocations and sub-structures, (c) g grains distributed within lamellar colony and sub-
structure in g grains, (d) a2/g lamellar and g grains, (e) recovered grains and (f) recrystallized g grains and a2 grains.

temperatures is shown in Fig. 7. The tensile strength at ambient
temperature is improved significantly, due to the fine and ho-
mogenous duplex microstructure. The yield strength (YS) increases
from about 750 MPa to 962 MPa with the UTS from about 885 MPa
to 1174 MPa. The tensile properties at room temperature and 800
C
of the current as-rolled alloy compared with other high Nb con-
taining TiAl alloys are listed in Table 1. Its UTS is higher than the
762 MPa of the Ti-45Al-8.5Nb-(W, B, Y) alloy [4]. It is also higher
than the 815 MPa of the Ti-45Al-7Nb-0.3W alloy [8] and the
881 MPa for the Ti-46Al-9Nb alloy [11]. However, the cracks tend to
traverse the lamellar colony and bypass fine g grains due to the
obtained fine duplex microstructure at high temperature.
Compared to the near g microstructure of the Ti-45Al-8.5Nb-(W, B,
Y) alloy, the lamellar colonies can be effective barriers to crack
 H. Zhou et al. / Journal of Alloys and Compounds 695 (2017) 3495e3502 3501

Fig. 7. (a) tensile strength-strain curves of tensile tests conducted along the rolling direction and (b) fracture morphology of as-rolled alloy at 800
C.

Table 1
Microstructure and tensile properties compared with other as-rolled TiAl alloys with Nb content 7%.

Alloy Microstructure Total As-rolled Room temperature 800
C Reference

before rolling reduction microstructure
YS MPa UTS MPa d% YS MPa UTS MPa d%
Ti-45Al-7Nb 0.3W Near g 73% Near g 10 mm 780a 780a 560a 660a 62a [8]
61% 815a 815a 605a 715a 75a [8]
Ti-45Al-8.5Nb -(W, B, Y) Nearly lamellar 75% Near g 15 mm 668a 762a 1.5a 500a 530a 2a [4]
Ti-46Al-9Nb Near g Near g 5 mm 754a 881a 2.5a 380a 455a 78a [11]
Ti-44Al-8Nb -(W, B, Y) Nearly lamellar 85% Duplex 5.3 mm 962 1174 1.0 681 777 37 Current alloy
a
The value inferred from the tensile property figures.

propagation of the current alloy, resulting in the strengthening of
the alloy. Meanwhile, the tensile elongation (d) at room tempera-
ture increases from about 0.37% of the as-forged [15] to 1.01%. As
shown in Table 1, it is a little lower than the 1.5% of the Ti-45Al-
8.5Nb-(W, B, Y) alloy [4] and the 2.5% of the Ti-46Al-9Nb alloy
[11]. The high density of dislocations, substructures (Fig. 6(b))
generated from the hot pack rolling, and the short annealing
treatment affect the improvement of ductility at room temperature.
Further work is continuing on heat treatment for balancing the
tensile strength and ductility at room temperature, and will be
reported in due course.
At elevated temperatures, the current as-rolled alloy still ex-
hibits excellent strength. The UTS is as high as 953 MPa at 750
C,
and the failure strength still remains high above 770 MPa with the
37% ductility at 800
C. Its YS and UTS are both higher than that of
other high Nb containing TiAl alloys at 800
C in Table 1. Of course,
the ductility is lower than the 62e75% of alloys in Table 1, which is
ascribed to the near g microstructure [16]. When temperature be-
comes as high as 850
C, the failure strength still remains higher
than 630 MPa with a good elongation value of above 45%. Even up
to 900
C, the as-rolled alloy displays a UTS value more than
450 MPa, showing a good retention of high temperature strength.
Many dimples are observed in Fig. 7(b), indicating that the brittle to
ductile transition of the current as-rolled alloy is between 750 and
800
C, while the Ti-45Al-8.5Nb-(W, B, Y) alloy is about 825
C [4]. It
is demonstrated that the present alloy is safer than the Ti-45Al-
8.5Nb-(W, B, Y) alloy at high temperatures.
In summary, the as-rolled Ti-44Al-8Nb-(W, B, Y) alloy exhibits a
failure strength of 1174 MPa, with 1.01% ductility at room temper-
ature. The failure strength still remains high above 950 MPa at
750
C, and the UTS is higher than 630 MPa at 850
C. The high
performance property sheet contains fine and homogenous duplex
microstructure with mean grain sizes of 5.3 mm, which was ob-
tained within six passes to a total thickness reduction of 85% by hot
pack rolling. A reduction of up to 25% per pass was ascribed to the
70% vol. % of disordered a phases. These a laths are converted by
repeated deformation into fine recrystallization and recovery sub-
grains. Then, both a / a2 ordering transformation and a/ a2/g
lamellar colony take place during cooling. Furthermore, the
occurrence of recrystallization and recovery of g phases results in
the refinement of the microstructure. As deformation proceeds
during the subsequent hot pack rolling, the fine duplex micro-
structure was obtained by repeated recrystallization, recovery and
phase transformation.
Acknowledgements
This work was financially supported by the National Nature
Science Foundation of China (Project No. 51471056) and the State
Key Laboratory for Advanced Metals and Materials foundation
(Project No. 2016-ZD01).
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