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Department of Materials Science and Engineering, Pohang University of Science and Technology, San 31, Hyoja-dong, Nam-gu, Pohang, Gyungbuk 790-784, Republic of Korea
Air Force Research Laboratory, AFRL/RXLM, Wright-Patterson AFB, OH 45433-7817, USA
a r t i c l e
i n f o
Article history:
Received 6 January 2010
Received in revised form 14 April 2010
Accepted 27 April 2010
Keywords:
Titanium alloy
Superplasticity
Dynamic globularization
Coarsening
Deformation mechanism
a b s t r a c t
The low-temperature superplasticity and dynamic coarsening behavior of Ti6Al2Sn4Zr2Mo0.1Si
were established and interpreted in the context of inelastic-deformation theory. The starting microstructure with an equiaxed-alpha particle size of 13 m was rened to 2.2 m by a treatment comprising
beta annealing/water quenching followed by warm rolling at 775 C. A series of tension and loadrelaxation tests were carried out for the coarse and ne microstructures at strain rates of 104 to 102 s1
in the temperature range of 650750 C. The ne microstructure exhibited enhanced superplasticity
(382826% elongation) compared to that of the coarse microstructure (189286% elongation); this trend
was attributed to a larger fraction of boundary sliding and lower friction stress for the ner material.
With respect to microstructure evolution, the coarsening rate of the alpha particles during deformation
was 12 times faster than that during static coarsening. Furthermore, both the static and dynamic coarsening rates for the Ti6Al2Sn4Zr2Mo0.1Si were 2.74.7 times lower than those for the Ti6Al4V,
a trend attributable to the lower diffusivity of Mo compared to that of V at a given test temperature. The
plastic ow behavior of the coarse and ne microstructures was rationalized in terms of microstructure
evolution during deformation.
2010 Elsevier B.V. All rights reserved.
1. Introduction
Alpha/beta titanium alloys are widely used for aerospace applications due to their high specic strength, excellent corrosion
resistance, and high-temperature properties [1]. For example,
Ti6Al2Sn4Zr2Mo0.1Si (Ti6242Si) has been used for jet engine
compressor disks because of its superior creep resistance and
higher service temperature (550 C) compared to the more common Ti6Al4V alloy [1,2].
With the application of net-shape processes such as isothermal
forging of billet and superplastic forming of sheet, cost savings
associated with improved material utilization can be achieved.
Despite this commercial benet, the widespread application of
such processes may be limited by processing requirements such
as high temperature (900 C) and/or low strain rate (103 s1 )
[3,4]. On the other hand, enhanced die-ll capacity/superplasticity
can be realized at lower temperatures (750 C) and/or higher
strain rates (102 s1 ) by rening the microstructure via severe
plastic deformation (SPD) methods such as high pressure torsion
(HPT), equal-channel angular extrusion (ECAE), and accumulative roll bonding (ARB) [59]. Other efforts have been made to
Corresponding author. Tel.: +82 54 279 2141; fax: +82 54 279 2399.
E-mail address: cslee@postech.ac.kr (C.S. Lee).
0921-5093/$ see front matter 2010 Elsevier B.V. All rights reserved.
doi:10.1016/j.msea.2010.04.082
achieve enhanced superplasticity utilizing dynamic globularization of a ne lamellar microstructure, i.e., the conversion of a
transformed-beta microstructure to a ne equiaxed microstructure
[1013].
To maintain superplastic characteristics to large strains,
microstructural coarsening must be limited during deformation. In this regard, the static and dynamic coarsening
behaviors of Ti6Al4V with an ultrane-grain (UFG) microstructure have recently been interpreted in terms of a modied
LifshitzSlyozovWagner theory by Semiatin et al. [14,15]. In
related work, Sargent et al. [16] have emphasized the importance
of the alpha particle size rather than the size of alpha subgrains or
beta grains to describe the superplastic ow of the UFG Ti6Al4V.
Although this previous research provides insight into the interaction of microstructure evolution and plastic ow in alpha/beta
titanium alloys, it is unclear how solutes other than vanadium
and aluminum may affect such phenomena. The objectives of the
present work, therefore, were to demonstrate a processing method
to achieve enhanced superplasticity in another alloy in this class,
i.e., Ti6242Si, and to establish the effect of a different solute, molybdenum, whose diffusivity is noticeably slower than vanadium, on
microstructure evolution. For this purpose uniaxial and stressrelaxation tests were conducted on sheet samples. The plastic ow
observations were analyzed in the context of inelastic-deformation
theory to determine the relative contributions of grain-matrix
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C.H. Park et al. / Materials Science and Engineering A 527 (2010) 52035211
(1)
= a + + g
(2)
The variables I and F represent the internal stress due to a longrange interaction force among dislocations and the friction stress
due to a short-range interaction between the lattice and a dislocation, respectively; a denotes the co-rotational material time rate of
an internal strain tensor, while and g are the plastic strain rate
due to GMD and GBS, respectively. At elevated temperature, F is
generally very small compared to I , and a is negligible for loadrelaxation tests under a steady-state condition, thus providing a
relatively simple constitutive equation consisting of only the and
g elements. Thus, two separate constitutive equations describing
GMD and GBS can be expressed in the following form similar to
that suggested by Lee and Hart [18].
I
g
g 0
= exp
p
=
(3)
1/Mg
temperature: 1005 C) and water quenched to obtain a martensitic microstructure with laths 0.2-m thick (Fig. 2b). The
microstructure was converted to a ne, equiaxed one via dynamic
globularization [10,1923] during warm cross-rolling at 775 C
using 10% reduction per pass to a total reduction of 80%. The rolling
process comprised two passes with a rolling direction parallel to
the length of the preform and the remaining passes parallel to the
width. The rolled sheet was water quenched following the last pass.
By this means, Ti6242Si with ne alpha particles (approximately
one-half of which were still somewhat elongated) that were separated by thin layers of the beta phase were produced (Fig. 2c). An
electron-backscatter-diffraction (EBSD) inverse-pole-gure map
for the alpha phase (showing boundaries with misorientation angle
15 ) revealed that the particle size was 2.2 m (Fig. 2d).
The low-temperature superplasticity and dynamic coarsening
behavior of Ti6242Si with the coarse and ne microstructures were
quantied via uniaxial-tension and load-relaxation tests. Tension
specimens with a gauge length of 5 mm and width of 2.5 mm
were machined parallel to the nal rolling direction of the plate.
To prevent oxidation of the surface (which can have a deleterious effect on superplasticity [24]), each specimen was coated
with Deltaglaze 151 (Acheson Colloids, Port Huron, MI). They
were tested under constant-crosshead-speed conditions using an
INSTRON 1361 screw-driven machine at homologous temperatures of 0.470.53 (650750 C) and nominal strain rates of 104
to 102 s1 . Load-relaxation tests were performed at 650750 C
using specimens with a gauge length of 25 mm. The load-time
data from the load-relaxation tests were converted to stress-vsstrain-rate plots using the relations suggested by Lee and Hart
[18], i.e.,
(4)
Fig. 1. Rheological description of an internal-variable model consisting of grainmatrix deformation (GMD) and grain-boundary sliding (GBS).
=
P{l0 + (x P/C)}
A0 l0
P
C{l0 + (x P/C)}
(5)
(6)
in which P and P denote the load and its time derivative, respectively, A0 and l0 are the cross-sectional area and the length of the
gauge section, respectively, x is the crosshead displacement, and
C is the machine stiffness (P/x for high stiffness machine such as
INSTRON 1361).
To compare the dynamic and static coarsening behaviors of the
present material, static heat treatments were also conducted at
750 C for 6, 24, 48 and 70 h followed by water quenching.
Microstructures were examined via optical metallography
(OM), scanning electron microscopy (SEM), transmission electron
microscopy (TEM), and EBSD analysis. For OM and SEM, Krolls
reagent (5% HNO3 , 10% HF, and 85% H2 O) was used to etch specimens. Backscattered electron images (BSEI) were taken in a JEOL
high resolution SEM, JSM-7401F. Thin foils for TEM were prepared by twin-jet electropolishing at 40 C using a mixture of
5% H2 SO4 and 95% CH3 OH. TEM micrographs were obtained by
utilizing a Cs corrected HR-STEM, JF-2200 (JEOL) operating at an
accelerating voltage of 200 kV. To measure the alpha particle size,
EBSD maps for the alpha phase were constructed using TSL software with a tolerance angle of 15 . Initially, the EBSD specimens
were electropolished using a LectroPol-5 (STRUERS) operated at a
voltage of 22 V for 25 s in a solution of 410 ml methanol, 245 ml
2-butoxy ethanol, and 40 ml 60%-HClO4 . EBSD was performed in
a Helios NanoLabTM 600 scanning electron microscope with an
accelerating voltage of 30 kV and a step size of 0.08 m. The condence index of the EBSD orientation measurements was between
0.29 and 0.64.
C.H. Park et al. / Materials Science and Engineering A 527 (2010) 52035211
5205
Fig. 2. Micrographs of the Ti6242Si program material: (a) as-received microstructure (OM), (b) martensitic structure after beta annealing and water quenching (TEM), (c)
dynamically globularized microstructure (backscattered electron image; the dark phase is alpha and the lighter phase is beta), and (d) dynamically globularized microstructure
(EBSD map for the alpha phase using a tolerance angle of 15 ).
4. Results
4.1. Uniaxial-tension ow behavior and elongation to failure
True stress-vs-strain curves for the CP (coarse-particle) and
FP (ne-particle) Ti6242Si materials (e.g., results for 750 C in
Fig. 3a and b) exhibited noticeable differences in terms of their
strain-rate and temperature dependences. The curves denoted
with open symbols in Fig. 3 comprise those determined directly
from the load-stroke measurements obtained during the constantcrosshead-speed tests. A more appropriate comparison of true
material behavior was obtained by estimating the constantstrain-rate ow response by compensating for the continuously
decreasing strain rate imposed during the tension tests. For this
v)m in which
purpose, each stress data point was multiplied by (h/
is the nominal strain rate, h is the instantaneous length of the
Fig. 3. True stress-vs-true strain curves measured at 750 C and various strain rates for (a) CP (13 (m) and (b) FP (2.2 (m) Ti6242Si specimens. The strain-rate dependence
of the strain-rate sensitivity (m) determined from load-relaxation tests is shown in (c).
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C.H. Park et al. / Materials Science and Engineering A 527 (2010) 52035211
mated from the load-relaxation data, whose strain rates span those
imposed during the uniaxial-tension tests (Fig. 3c). The corrected
(constant-strain-rate) true stress-vs-strain curves for the CP and FP
Ti6242Si materials (closed symbols in Fig. 3a and b) also showed
a noticeable dependence on strain rate. For example, the peak
stresses of the CP specimens were considerably higher than those
of the FP specimens at the same test condition, and the ow stresses
of both materials decreased with decreasing strain rate from 102
to 104 s1 . Furthermore, it is of interest to note that the FP material
exhibited considerable ow hardening at a strain rate of 104 s1 ;
this latter observation behavior will be discussed in the context of
the corresponding microstructural evolution in Section 5.3.
The elongations of the CP specimens (81286%) were considerably less than those of the FP samples (382826%) tested at the
same strain rate and temperature (Fig. 4). For instance, the elongation (expressed as a true strain) of the CP sample deformed at 750 C
and 104 s1 was 1.3, while that of the corresponding FP specimen
was 2.3. Fig. 5a summarizes the total elongations for the CP and
FP specimens tested at various temperatures and strain rates as
well as previously reported results obtained under conventional
(higher-temperature) superplastic conditions [4]. Two aspects can
be noted in this plot. First, the FP material exhibited approximately
2.5 times larger total elongations compared to those for CP material in the temperature range of 650750 C. Second, despite the
difference in phase volume fractions, the total elongations for FP
specimens deformed at 750 C were similar to those for the conventional material tested at the much higher temperature of 940 C
[4]. The high elongation of the FP Ti6242Si can be attributed to
the operation of phase-boundary sliding even at 750 C, as will be
discussed in Section 5.1. Such a conclusion is supported by values
of the strain-rate sensitivity (m) of the CP and FP materials estimated from load-relaxation tests. The FP microstructure showed
substantially higher ms at both test temperatures and each strain
rate (Fig. 3c). Because maximum elongation is usually found for
test conditions having the highest m value, it is not surprising to
observe the largest total elongation for the FP microstructure for
tests at 750 C, 104 s1 , i.e., 826%.
4.2. Load-relaxation behavior
The stress-vs-strain-rate data obtained from the load-relaxation
tests (data points, Fig. 6) were used to quantify and interpret
Fig. 6. Comparison of experimental ow stress-vs-strain-rate data obtained by load-relaxation tests () and predicted curves based on the internal-variable theory of
inelastic deformation (lines). The alpha particle sizes and test temperatures were (a) 13 (m and 650 C, (b) 13 (m and 750 C, (c) 2.2 (m and 650 C, and (d) 2.2 (m and 750 C,
respectively.
C.H. Park et al. / Materials Science and Engineering A 527 (2010) 52035211
5207
Table 1
Constitutive parameters for CP and FP Ti6Al2Sn4Zr2Mo0.1Si materials determined from load-relaxation tests.
Material
Temperature ( C)
GMD parameters
GBS parameters
log *
log
log g
log g 0
Mg
CP (d = 13 m)
650
750
3.01
2.91
4.46
2.01
0.15
0.15
1.99
1.04
7.02
6.30
0.5
0.5
FP (d = 2.2 m)
650
750
3.32
3.01
1.72
1.30
0.15
0.15
1.38
0.85
6.25
6.21
0.5
0.5
(7)
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C.H. Park et al. / Materials Science and Engineering A 527 (2010) 52035211
Fig. 7. EBSD inverse-pole-gure maps (tolerance angle = 15 ) for FP specimens deformed at 750 C and 104 s1 for (a) 5 h, (b) 10 h, (c) 15 h and (d) 21 h. The four EBSD maps
at the bottom are for FP specimens statically annealed at 750 C for (e) 6 h, (f) 24 h, (g) 48 h and (h) 70 h, respectively.
Table 2
Comparison of the values of the coarsening-rate constant K for alpha particles in Ti6Al2Sn4Zr2Mo0.1Si and Ti6Al4V.
Material
Temperature ( C)
Ti6242Si
Ti64
750
775
0.12
0.56 [30]
1.43
3.9 [30]
C.H. Park et al. / Materials Science and Engineering A 527 (2010) 52035211
5209
Fig. 8. Relative contribution of GMD and GBS to the overall deformation for CP and
FP Ti6242Si at temperatures of 650 and 750 C and a strain rate of 104 s1 .
(8)
18, 520
T (K)
17, 460
T (K)
(9)
(10)
Eqs. (9) and (10) indicate that the diffusivity of the Mo solute in the
beta matrix for the Ti6242Si is approximately one-sixth that of V in
Ti6Al4V alloy at the same temperature (Table 2). Thus, the lower
dynamic and static coarsening rates of the Ti6242Si compared to
those of Ti6Al4V can be explained at least qualitatively to be a
result of differences in the diffusivity of the rate-limiting solute.
5.3. Effect of microstructure evolution on plastic ow
The 104 s1 true stresstrue strain curves adjusted for a constant strain rate (closed symbols in Fig. 3a and b) exhibited near
steady-state ow for CP samples and ow hardening for FP specimens. These observations can be rationalized in the context
of recent research on the superplastic ow behavior of twophase Ti alloys [30]. In this former work, the instantaneous ow
response was related to the evolving microstructure using the
BirdMukherjeeDorn generalized constitutive equation [35], viz.,
=
ADGb n b p
kT
(11)
Fig. 9. The coarsening behavior of FP specimen under dynamic ( = 104 s1 ) and static conditions at 750 C. The experimental data were t with n equal to (a) 2, (b) 3,
or (c) 4.
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C.H. Park et al. / Materials Science and Engineering A 527 (2010) 52035211
following relationship:
=
0
d p/n
(12)
d0
3 [0.3287/3 (1 + 1 0.7634/3 ) ]
vd
=
4[((2(1 + ))/(3(0.5 0.5731/3 )) + (0.51/3 + 0.6652/3 )/(3(0.143 + 0.9341/3 ))]
=
=
w
u
+ 0.5
u3 RT
D CF VM
(13a)
(13b)
(13c)
Acknowledgement
This work was supported by a grant from the US Air Force Ofce
of Scientic Research and its Asian Ofce of Aerospace Research
and Development (Dr. J.P. Singh, program manager).
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