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Materials and Design 46 (2013) 38–48

Contents lists available at SciVerse ScienceDirect

Materials and Design


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

An experimental study of deformation mechanism and microstructure


evolution during hot deformation of Ti–6Al–2Zr–1Mo–1V alloy
D. He a,b, J.C. Zhu a,⇑, Z.H. Lai a, Y. Liu a, X.W. Yang a
a
National Key Laboratory for Precision Hot Processing of Metals, Harbin Institute of Technology, Harbin 150001, China
b
State Key Laboratory of Nonlinear Mechanics, Institute of Mechanics, Chinese Academy of Sciences, Beijing 100190, China

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

Article history: Isothermal tensile tests have been performed to study the deformation mechanisms and microstructure
Received 11 March 2012 evolution of Ti–6Al–2Zr–1Mo–1V titanium alloy in the temperature range 750–850 °C and strain rate
Accepted 26 September 2012 range 0.001–0.1 s1. The deformation activations have been calculated based on kinetics rate equation
Available online 11 October 2012
to investigate the hot deformation mechanism. Microstructures of deformed samples have been analyzed
by electron backscatter diffraction (EBSD) to evaluate the influences of hot deformation parameters on
Keywords: the microstructure evolution and recrystallization mechanism. The results indicate that deformation
Deformation mechanism
mechanisms vary with deformation conditions: at medium (800 °C) and high (850 °C) temperature, the
Recrystallization mechanism
Microstructure globularization
deformation is mainly controlled by the mechanisms of dislocation creep and self-diffusion, respectively.
Electron backscatter diffraction The microstructure globularization mechanisms also depend on deformation temperature: in the tem-
Titanium alloys perature range from 750 to 800 °C, the high angle grain boundaries are mainly formed via dislocation
accumulation or subgrain boundaries sliding and subgrains rotation; while at high temperature of
850 °C, recrystallization is the dominant mechanism. Especially, the evolution of the recrystallization
mechanism with the deformation temperature is first observed and investigated in TA15 titanium alloy.
Ó 2012 Elsevier Ltd. All rights reserved.

1. Introduction activation [7], are not only influenced by the alloying elements [8]
and initial microstructure [9], but also depended on the deforma-
TA15 titanium alloy with a nominal composition of Ti–6Al–2Zr– tion temperature, strain and strain rate [10,11]. On the other hand,
1Mo–1V, is developed on the basis of Russia alloy BT20 [1]. As a the microstructure evolutions, e.g. a M b phase transformation, a
classic near a titanium alloy, TA15 is an ideal high-temperature lamellae globalization, grain coarsening and recrystallization nuclei
alloy since it combines the excellent creep behavior of a titanium and their growth, are also complex and significantly affected by hot
alloys with the high strength of a + b titanium alloys [2]. Therefore, deformation parameters [12,13]. This implies that a strong interac-
TA15 is preferentially used in aerospace field in China to produce tion relationship between the microstructure evolution and hot
the compressor blades, compressor disks of gas turbine engine deformation behavior/mechanism exists during hot deformation
and large front fans of modern jet engines [3]. process [14]. Therefore, the study of hot deformation mechanism
Generally, because of high yield strength and relatively low and microstructure evolution is very important and has attracted
elastic modulus, the fabrication and forming operation of TA15 more and more researchers’ attentions.
titanium alloy are usually conducted at elevated temperature, such With regard to hot deformation behavior and mechanism, many
as a + b forming (deformed in the temperature range 30–200 °C studies have been carried out on titanium [7,15] and titanium
below the b-transus), b deforming (deformed at a temperature alloys [8,11–13] by combining compressive or tensile deformation
above the b-transus) [4,5]. On the other hand, since TA15 alloy is behavior with thermal activation energy analysis. However, up to
close to single phase, the influence of traditional heat treatment now, only a few studies have been conducted on the hot deforma-
on the microstructure is not as obvious as that for other metal tion mechanism of near a titanium. Especially, for TA15 titanium
alloys, e.g. steels. Therefore, thermomechanical processing is usu- alloy, although the microstructure evolution and mechanism prop-
ally adopted to control both the shape size and the microstructure erties of TA15 titanium alloy under multi-step local loading form-
morphology/composition of the near a titanium alloy part [6]. ing have been studied by Sun et al. [16], the deformation
Recent research results indicate that the hot deformation mech- mechanisms are roughly summarized as dynamic recrystallization
anisms of titanium alloys, which are generally controlled by thermal according to the peak and steady status phenomenon of flow stress
curves or the appearance of equiaxed a grains. Obviously, they are
⇑ Corresponding author. Tel.: +86 451 86413792; fax: +86 451 86413922. not enough for us to deeply understand the hot deformation mech-
E-mail address: [email protected] (J.C. Zhu). anisms and the microstructure evolutions. Taking the appearance

0261-3069/$ - see front matter Ó 2012 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.matdes.2012.09.045
D. He et al. / Materials and Design 46 (2013) 38–48 39

of equiaxed a grains for example, many hypotheses could account second a lamellae (as) and a few retained b phase (body-centered
for it, e.g. laths shearing and interfaces migration by diffusion [17], cubic, bcc) layer (br), as shown in Fig. 1. The average size of primary
DDRX [18], CDRX [19], rotational dynamic recrystallization (RDRX) a lamellae is 10 lm in thickness and 35–40 lm in length; while for
[20] and geometric dynamic recrystallization (GDRX) [21,22]. second a lamellae, the values are 2–2.5 lm and approximately
The objective of the current work is focused on the hot deforma- 15 lm, respectively.
tion mechanism and microstructure evolution of TA15 titanium al- Flat tension samples of 49 mm length and 2 mm thickness were
loy in the deformation temperature range of 750–850 °C and strain machined along the elongated direction from the mentioned TA15
rate range between 0.001 and 0.1 s1. The rest of the paper is ar- titanium alloy wrought bars, as shown in Fig. 2. It is noteworthy
ranged as follows. Firstly, tensile tests have been performed under that the non-standard tensile specimens were used in the tensile
different considerations; then, the deformation behaviors and deformation experiment. This is because that we are focused on
mechanisms have been evaluated based on the obtained stress– the deformation mechanism and microstructure evolution during
strain curves and calculated deformation activations. Subsequently, hot tensile deformation process but not on the standard high tem-
microstructure evolutions have been deeply investigated by combi- perature tensile mechanical properties (e.g. tensile strength, yield
nation of electron backscatter diffraction (EBSD) technique. Finally, stress and elongation) of this material in the current study. The
the deformation mechanism, a lamellae globalization, recrystalliza- tensile deformation were carried out in a high-temperature tensile
tion mechanism and their evolutions depending on deformation testing machine (INSTRON 5500R) at three temperatures (750, 800
conditions have been further discussed and summarized. and 850 °C) and three constant strain rates (0.001, 0.01, 0.1 s1),
respectively.
In order to take the influence of deformation strain into consid-
2. Experimental procedure eration, the tensile tests stop at different strains, i.e. 0.02 or 0.04,
0.10, 0.20, respectively. The detailed parameters are listed in Table
2.1. Materials and sample preparation 2. All specimens were mounted on the holder when the furnace
temperature reaching to the given temperature and then heated
The chemical composition of used TA15 titanium alloy is given to test temperature again. All specimens were held for 3 min at test
in Table 1. The b-transus temperature of used TA15 alloy was temperature to improve the temperature uniformity of whole spec-
993 °C. The initial microstructure consisted of coarse primary a imen and then deformed to given strain. After tensile deformation,
phase (hexagonal close-packed, hcp) lamellae (ap), relatively fine the specimens were quenched in cold water immediately in order to
maintain the microstructure characteristics at high temperature.
Table 1
Chemical composition of used TA15 alloy (mass fraction, %).
2.2. EBSD measurement and microstructure analysis
Al Zr Mo V Fe Ti
6.47 1.59 1.45 1.91 0.038 Bal. Microstructure and local crystallographic orientations of de-
formed samples were examined by EBSD techniques. For this

Fig. 1. Initial microstructure of used TA15 titanium alloy. (a) Photo of the metallographic structure, (b) inverse pole figure colored map, map color code: Z direction, scanning
step size: of 0.2 lm.

Fig. 2. The sketch map of tensile sample machining, geometry of the tensile sample and sample photo after tensile deformation.
40 D. He et al. / Materials and Design 46 (2013) 38–48

Table 2 @ ln r
Detailed parameters for tensile deformation test. m¼ ð3Þ
@ ln e_ T
Test no. Deformation strain Strain rate (s1) Temperature (°C)
where m represents the strain-rate sensitivity of flow stress, m = 1/
1/2/3 0.02/0.10/0.19 0.001 750
n.
4/5/6 0.04/0.10/0.19 0.01 750
7/8/9 0.04/0.10/0.19 0.1 750 When e_ is constant, Q also can be derived from Eq. (2) and
10/11/12 0.02/0.10/0.19 0.001 800 written as:
13/14/15 0.04/0.10/0.19 0.01 800
16/17/18 0.02/0.10/0.19 0.1 800 1 @ ln r
Q ¼R ð4Þ
19/20/21 0.02/0.10/0.19 0.001 850 m @ lnð1=TÞ e_
22/23/24 0.04/0.10/0.19 0.01 850
25/26/27 0.04/0.10/0.19 0.1 850 The values of calculated n and Q under different deformation
conditions are listed in Table 3. The results show a good agreement
purpose, the flat surfaces of tensile samples were prepared through with research work of others under certain conditions, i.e. when
standard grinding and polishing routines (ASTM: ASTM E3-11). The the titanium or titanium alloys were deformed at low temperature
final polishing with a polishing solution consisting of colloidal sil- (here, less than 850 °C for TA15) and low strain rate (less than
ica (OP-S, 90 vol.%) and H2O2 (10 vol.%) was performed. Long time 0.1 s1) [8,26–28]. It can be seen that the values of calculated n
(30 min) for final polishing is to minimize the strain caused by the are temperature-dependent (decreased from 7.28 to 3.86) in the
grinding and polishing processes. temperature range 750–850 °C. Similarly, the activation energy Q
EBSD measurements were carried out on a JEOL 6500F scanning also decreases from 697.44 to 163.28 kJ mol1 as the temperature
electron microscope equipped with an EBSD system developed by increases from 750 to 850 °C. The obvious variations of calculated n
EDAX/TSLÒ. In order to facilitate comparison, the central region of and Q further indicate that different deformation mechanisms may
each tensile deformed specimen was selected for EBSD mea- exist in the temperature range 750–850 °C at low strain rate.
surements (see the blue1 region in Fig. 2). The grain size and mor-
phology, crystal orientations, grain or subgrain boundaries and 3.3. Grain morphology and size evolution
such other microstructure characteristics were processed and ana-
lyzed by the EDAX-TSL OIM™ 5.4 software. Before analyzing the grain morphology and size evolution dur-
ing tensile deformation, we must note that three temperatures
3. Results (750, 800 and 850 °C) were used in this study. The microstructures
of samples at three test temperatures but without any tensile
3.1. Tensile deformation behavior deformation were given by Fig. 4. Obviously, the microstructure
of samples at three different temperatures (i.e. 750, 800 and
The tensile load–displacement curves of TA15 titanium alloy 850 °C) are similar: all of them are composed of thick primary a
achieved by isothermal tensile test under different deformation lamellae (ap), some coarse equiaxed a grains and a few retained
conditions are shown in Fig. 3. The results indicate that the tensile b phase. With the increasing of temperature, the thickness of a
load decreases with the increase of deformation temperature and lamellae increases slightly: its mean value increases from 6.9 lm
decrease of strain rate. Generally, the tensile load rapidly increases at 750 °C to 8.1 lm at 850 °C. Furthermore, the volume fraction
to a peak, then starts to decrease continuously, and finally attains a of equiaxed a grains also increases as the temperature increases,
steady state. Such tensile deformation behavior is usually consid- as shown in Fig. 4c. This is mainly resulted by the coarsening and
ered as a characteristic for hot working accompanied by dynamic ripening effects of some short or small a grains at higher temper-
recrystallization (DRX) [23,24]. ature (i.e. 850 °C at here).
Although the microstructures at different temperatures are lit-
3.2. Kinetic analysis tle different, they will not significantly affect the following recrys-
tallization mechanism studies. This is because that we are focused
As mentioned in the introduction, the high temperature defor- on the evolutions of ‘‘newly formed’’ small and equiaxed a grains
mation behavior of alloys is mainly controlled by thermal activa- but not on the original coarse microstructure. Furthermore, when
tion [8]. Commonly, the temperature and strain rate dependence we study the influences of tensile strain or strain rate on the evo-
of flow stress in hot deformation can be described by Arrhenius lution of microstructure, the results from the samples deformed at
kinetic rate equation given by [25,26]: different strains or strain rates but at same given test temperature,
  are compared and analyzed.
Q The microstructures of the TA15 titanium alloy after tensile
e_ ¼ Arn exp  ð1Þ
RT deformation (e ¼ 0:19) at strain rate of 0.01 s1 and in temperature
where e_ is the strain rate (s1), A is a material constant, r is the flow range 750–850 °C are presented as a unique color map in Fig. 5.
stress (MPa), n is the stress exponent, Q is the activation energy It is obvious that the microstructure evolution is strongly
(kJ mol1), R is the gas constant, and T is the temperature in Kelvin dependent on deformation temperature. At low temperature
(K). (750 °C), although a lot of equiaxed a grains are observed, there
To facilitate obtaining the kinetic parameters n and Q, the are still a certain number of a lamellae, as seen from the top region
Eq. (1) can be written as: in Fig. 5a. With increasing deformation temperature, the lamellae
globalization process is smoothly developed: the fractions (in grain
lnðe_ Þ ¼ lnðAÞ þ n lnðrÞ  Q =ðRTÞ ð2Þ numbers) of equiaxed a grains (aspect ratio less than 2) increase to
Thus, when T is constant, one defines, from Eq. (2). 67% and 85% at 800 and 850 °C, respectively. Few a lamellae
appear at the strain of 0.19 and temperature of 850 °C, as shown
in Fig. 5c.
Besides of the obvious lamellae globalization, the average grain
size also decreased from 9.43 lm to 2.5 lm (in diameter) as the
1
For interpretation of color in Figs. 1, 2, 4–12 the reader is referred to the web temperature increased from 750 to 850 °C. This result is mainly
version of this article. caused by the increase in the number of ‘‘new’’ grains with small
D. He et al. / Materials and Design 46 (2013) 38–48 41

Fig. 3. Tensile load–displacement curves under various deformation conditions during hot tensile deformation. (a) 750 °C, (b) 800 °C, and (c) 850 °C.

boundaries (indicated by black line) and some of them even


Table 3 formed a ‘‘necklace structure’’, which is usually identified as one
Values of calculated n and Q under different deformation conditions.
of characteristics of recrystallization [23,29,30].
Deformation conditions n Q (kJ mol1)
1
Strain rate (s ) Temperature (°C)
3.4. Grain and subgrain boundary structure evolution
0.001–0.1 750 7.28 697.44
800 5.26 357.87
850 3.86 163.28
The grain-subgrain boundary (GSB) evolutions with increasing
deformation strain at different temperatures and deformation
strains are shown in Figs. 7–9. In these GSB maps, the red, green
size. The distribution maps of grains with diameter less than 4 lm and blue lines represent the low angle boundaries (<5°) (LAB),
are shown in Fig. 6. Obviously, the number of small ‘‘new’’ grains medium angle boundaries (between 5° and 15°) (MAB) and high
(color grains) increased with increasing deformation temperature. angle boundaries (>15°) (HAB), respectively. No twin boundaries
These small ‘‘new’’ grains distributed along the original grain are detected under all test conditions.

Fig. 4. Original microstructures (before tensile deformation) displayed as inverse pole figure (IPF) colored map of TA15 titanium alloy with 3 min holding at different
temperatures, color code: Z direction; scanning step size: 0.1 lm. (a) 750 °C, (b) 800 °C, and (c) 850 °C.
42 D. He et al. / Materials and Design 46 (2013) 38–48

Fig. 5. Microstructures displayed as unique color maps of TA15 titanium alloy deformed at a strain rate of 0.01 s1 to a strain of 0.19 at: (a) 750 °C, (b) 800 °C, and (c) 850 °C.

Fig. 6. Combination map of grain boundary and small grains (less than 4 lm in diameter, colored according to inverse pole figure color) of TA15 titanium alloy deformed at a
strain rate of 0.01 s1 to a strain of 0.19 at: (a) 750 °C, (b) 800 °C, and (c) 850 °C.

At temperature of 750 °C, the total density of subgrain bound- as shown in Fig. 7(a–c), respectively. Most of the new formed HABs
ary (less than 15°) (SB) is relatively low and its distribution is het- distribute along the original coarse grain boundaries. However,
erogeneous at strain 0.04, as shown in Fig. 7a. A lot of equiaxed they are usually accompanied with high density of SBs, as seen
grains containing few SBs are detected in the top region of from the magnification maps in Fig. 7(b and c).
Fig. 7a. The results analysis shows that these equiaxed grains usu- When the tensile deformation temperature increased to 800 °C,
ally have a high Schmid factor value (larger than 0.4) for basal slip some new grains containing few subgrain boundaries appear along
systems. However, almost all of the lamellae in the half bottom re- the original coarse grain boundaries, as seen from the magnifica-
gion contain a high density of SBs. In this zone, most of grains have tion maps in Fig. 8(b and c). With increasing tensile strain, the
a low Schmid factor values (less than 0.1) for basal slip systems. number of new grains increased steadily, i.e. the new grains with
With increasing strain, the evolution of grain and subgrain struc- HABs distributes along the original grain and a ‘‘necklace
ture is very obvious. The densities of new formed HABs increase structure’’ was formed, as seen from the magnification map in
dramatically as the strains increase from 0.04 to 0.10 and 0.20, Fig. 8c.

Fig. 7. GSB maps of TA15 titanium alloy obtained at 750 °C and at a strain rate of 0.01 s1 to a strain of: (a) 0.04, (b) 0.10, and (c) 0.20; red lines correspond to low angle
boundaries (<5°), green lines to grain boundaries between 5° and 15°, blue lines to high angle boundaries (>15°).
D. He et al. / Materials and Design 46 (2013) 38–48 43

Fig. 8. GSB maps of TA15 titanium alloy obtained at 800 °C and at a strain rate of 0.01 s1 to a strain of: (a) 0.04, (b) 0.10, and (c) 0.20; red lines correspond to low angle
boundaries (<5°), green lines to grain boundaries between 5° and 15°, blue lines to high angle boundaries (>15°).

Fig. 9. GSB maps of TA15 titanium alloy obtained at 850 °C and at a strain rate of 0.01 s1 to a strain of: (a) 0.04, (b) 0.10, and (c) 0.20; red lines correspond to low angle
boundaries (<5°), green lines to grain boundaries between 5° and 15°, blue lines to high angle boundaries (>15°).

At a temperature of 850 °C, even at a low tensile deformation 3.5. Crystal orientation distribution and evolution
strain (e.g. e ¼ 0:04), a lot of new equiaxed grains formed by HABs
structures appeared along original grain boundaries, as shown the The crystal orientation distributions of small a grains (less than
magnification map in Fig. 9a. Furthermore, almost all of these new 2 lm in diameter) and original coarse a grains (larger than 6 lm in
equiaxed grains do not contain SBs. These new grains are identified diameter) for TA15 titanium alloy tensile deformed under different
as recrystallized grains. At this temperature, the classic ‘‘necklace conditions are presented in {0 0 0 1} and {1 1 2 0} pole figures, as
structure’’ is observed at all tested strains. The decrease of initial shown in Figs. 9–11 respectively.
grain size and the globalization are more and more obvious as At 750 °C, a strong corresponding relationship between the
the tensile strain increased from 0.04 to 0.2. crystal orientation of coarse a grains and small a grains exists,

Fig. 10. {0 0 0 1} and {1 1 2 0} pole figures of small grains (less than 2 lm in diameter, plotted by color intensity) and coarse original grains (large than 6 lm in diameter,
plotted by contour line) for TA15 titanium alloy deformed at a temperature of 750 °C and a strain rate of 0.01 s1 to a tensile strain of 0.20.
44 D. He et al. / Materials and Design 46 (2013) 38–48

Fig. 11. {0 0 0 1} and {1 1 2 0} pole figures of small grains (less than 2 lm in diameter, plotted by color intensity) and coarse original grains (large than 6 lm in diameter,
plotted by contour line) for TA15 titanium alloy deformed at a temperature of 800 °C and a strain rate of 0.01 s1 to a tensile strain of 0.20.

Fig. 12. {0 0 0 1} and {1 1 2 0} pole figures of small grains (less than 2 lm in diameter, plotted by color intensity) and coarse original grains (large than 6 lm in diameter,
plotted by contour line) for TA15 titanium alloy deformed at a temperature of 850 °C and a strain rate of 0.01 s1 to a tensile strain of 0.20.

i.e. some of them correspond well (indicated by black stars) and to find that, even in the narrow temperature range and at relatively
others keep a minor shift relationship (marked by dotted blue ar- low strain rate (0.001–0.1 s1), the deformation mechanisms of
rows). Furthermore, the crystal orientation distribution of small TA15 titanium alloy are various under different hot deformation
a grains shows a weak texture. conditions.
However, at the temperature of 800 °C, a much stronger depen- At low temperature (750 °C) and low strain rate (0.001–0.1 s1),
dent relationships between the crystal orientation of coarse a the calculated activation energy is 697 kJ mol1. Obviously, this va-
grains and small a grains is presented comparing with the situa- lue is much larger than the activation energy for self-diffusion of a-
tion at 750 °C, as shown in {0 0 0 1} and {1 1 2 0} pole figures in Ti (204 kJ mol1) [31] and b-Ti (153 kJ mol1) [32]. Furthermore,
Fig. 10(a and b), respectively. The corresponding EBSD data are the stress exponent value (7.28) is also far larger than those during
checked and the results show that almost all grains in the scanned deformation controlled by diffusion and dislocation [33].
region have a similar crystal orientation (close to Similar results on such high activation energy or stress expo-
(1 1 2 3)h8 5 5 3i direction) and high Schmid factors (lar- nent for titanium alloys have also been reported by other research-
ger than 0.35) for basal slip system. ers. The work of Li et al. showed that the activation energy was
When the deformation temperature increased to 850 °C (as 661.90 kJ mol1 during the hot compression of Ti–3Al–5V–5Mo
shown in Fig. 12), although there still exists a certain degree of titanium alloy in a + b phase region and the reasons for high acti-
dependent relationship between the crystal orientation of coarse vation energy were attributed to dynamical recrystallization. Sim-
a grains and small a grains, a relatively random crystal orientations ilarly, the results of Semiatin et al. [34] also showed that the
are also presented, i.e. the texture of small a grains (Max = 1.96 in activation energy was 700 kJ mol1 during the hot compression
{1 1 2 0} pole figure) is much weaker than other situations. deformation of Ti–6Al–4V with a lamellar colony microstructure
at 815–995 °C. They pointed out that the high activation energy va-
lue (700 kJ mol1) did not have a true physical significance but was
4. Discussion rather an artifact of the fitting of data for two-phase materials [34].
The calculated activation energy values of TC11 with lamellar
4.1. Hot deformation mechanisms microstructure were 601.12 kJ mol1 at low temperatures (890–
980 °C) and high strain rates (0.1–10 s1) and 875.54 kJ mol1 at
From the results of flow stress behavior, calculated activation high temperature (995 °C) and high strain rates (0.1–10 s1),
energy and the evolution of grain/subgrain structures, it is obvious respectively [35]. The results were considered to be caused by
D. He et al. / Materials and Design 46 (2013) 38–48 45

the deformation twining and phase transformation during defor- apparent deformation activation energy of a-Ti (346 kJ mol1
mation, respectively. [35]). Therefore, the deformation is mainly controlled by the mech-
Actually, different researchers related such high deformation anism of dislocation creep under the above mentioned conditions.
activation energy to different reasons in addition to the dynami- However, it is worth noting that the obtained stress exponent
cally recrystallization, deformation twining and phase transforma- (n = 5.25) is still a little higher than other similar situations, e.g.
tion mentioned above, e.g. the effect of stress on activation energy 4.01 for TC11 compressed at strain rate 0.01 s1 and in the temper-
[25], and the globularization of lamellar microstructure [35]. ature range 890–980 °C [35], 3.3–3.6 for Ti–6Al–7Nb alloy in the
Because the a phase is ‘‘harder’’ than b, the deformation mainly temperature range 750–850 °C and strain rate range 0.001–10 s1
concentrated on b phase at the initial stage of deformation. The [37], 3.4 for Ti–6Al–4V with an equiaxed a + b microstructure in
heterogeneous deformation on a and b phase can lead to stress the limited strain rate range 0.0003–0.01 s1 and temperature
accumulation at the a/b interface [25]. In our current studied range 750–950 °C [26]. Here, the most possible reason accounting
material, although a phase take around 90% volume fraction, the for relatively high stress exponent is that the softening behavior
heterogeneous deformation on a and b phase and the main defor- (e.g. dynamic recrystallization, dynamic recover) is still weak at
mation strain is gradually moving to a phase with increasing medium temperature (800 °C) and low strain rate. Although the
deformation strain are also obvious. This process can be indirectly frequency of high angle misorientation (larger than 15°) at
validated by the evolution of grain boundaries with increasing 800 °C is higher than that at 750 °C, but it is still relatively low (less
strain, as shown in Fig. 7: the subgrain boundaries mainly distrib- than 50%) and significantly decreased with increasing tensile
uted at thin b layer or a/b interface at low strain (e.g. 0.04 and 0.10) strain, as seen in Fig. 13(a and b). The relatively low fractions of
but they gradually extend into the coarse a lamellae with increas- high angle grain boundaries indicate that the recrystallization is
ing strain. still incomplete.
In addition, the starting microstructure is also an important fac- When the deformation temperature increases to 850 °C, the
tor leading to high calculated activation energy. The results of rel- calculated activation energy and stress exponent values are 163.2
evant studies indicate that titanium alloys with lamellar a starting 8 kJ mol1 and 3.86, respectively. This activation energy value lies
microstructure usually have a relatively high activation energy va- between the activation energy values for self-diffusion of b-Ti
lue during hot deformation under certain conditions [25,35,36]. (153 kJ mol1) [32] and a-Ti (204 kJ mol1) [31]. These results
This result is usually attributed to globularization of the starting imply that with increasing temperature, the diffusion ability is
lamellar microstructure. The mechanisms of globularization will enhanced and the deformation mechanism is the dislocation move-
be discussed in the following subsection. ment controlled by self-diffusion.
At medium temperature (800 °C) and low strain rate (0.001– Furthermore, the stress exponent value (n = 3.86) is much lower
0.1 s1), the calculated activation energy is 357.87 kJ mol1. than that at 750 (n = 7.28) and 800 °C (n = 5.26). There are two pos-
Although it is far larger than the activation energy values for sible reasons accounting for it. Firstly, the softening behavior
self-diffusion of a-Ti (204 kJ mol1) [31] and b-Ti (153 kJ mol1) (recrystallization) is enforced at deformation temperature 850 °C.
[32], this value lies in the range of activation energy values for dis- A lot of new equiaxed a grains are observed along the original
location creep of a-Ti (200–360 kJ mol1 [35]) and is close to the coarse a grain boundaries, as shown in Fig. 9. At the same time,

Fig. 13. Relative frequency of misorientation for TA15 titanium alloy tensile deformed at a strain rate of 0.01 s1 as a function of strain and temperature: (a) 750 °C (b) 800 °C
(c) 850 °C.
46 D. He et al. / Materials and Design 46 (2013) 38–48

globular shape a grains are formed by the interfaces migration


which is driven by the urge to minimize the interfacial energy.
In our current presentation, at low temperature (i.e. 750 °C or
800 °C here), because the effect of recovery is still relatively weak,
the dislocations accumulate constantly along the planes of shear
with increasing strain. Obviously, the accumulation of dislocations
can lead to the transition of low angle grain boundaries into high
angle grain boundaries. On the other hand, the subgrain bound-
aries sliding and subgrains rotation to relieve the stress/strain con-
centration or to coordinate the deformation can also promote the
formation of high angle grain boundaries. Finally, the a lamellae
are decomposed into several short a grains by gradually formed
high angle grain boundaries.
Fig. 14. Schematic illustrating the steps of globularization process [33]. The processes of subgrain boundaries accumulation and the for-
mation of high angle grain boundaries within originally coarse a
lamellae interiors are shown in Fig. 15. Specially, the close crystal
the fraction of high angle grain boundaries (>15°) is around 60%. It orientation distribution of the selected equiaxed a grains (marked
is much higher than the values at 750 and 800 °C, as shown in by dotted black lines) which are adjacent to each other further val-
Fig. 13c. These results show that the recrystallization is enforced idate that these short a grains are formed by accumulation of dis-
and more sufficient at 850 °C. Secondly, with increasing tempera- locations along the planes of shear or subgrains rotation, as can be
ture, the fraction of soft and more easily deformed b phase [37] seen from the crystal orientation distribution presented in inverse
(comparing with a phase, hexagonal lattice) is increased gradually, pole figure in Fig. 15.
which also lead to the decrease of flow stress and the weakening of However, at higher temperature (i.e. 850 °C), the globulariza-
harden behavior. tion shows some different characteristics. The density of subgrain
boundaries (<15°) is much lower than situations at 750 and
4.2. Lamellae globularization 800 °C, as shown in Figs. 9 and 13c. The static results are also pre-
sented in Fig. 13. According to the previous discussion, this is
Lamellae globularization is widely observed in hot deformation mainly because the softening effect is pronounced at higher defor-
processes of titanium alloys and investigated by many researchers mation temperature (i.e. 850 °C here). Therefore, the original a
[17,25,26,34]. One widely accepted globularization mechanism lamellae cannot be easily decomposed by forming high angle grain
considers that the globularization consists of two events: shearing boundaries though the dislocation accumulation, which is the
of laths and formation of globules [17,25]. The detailed process was globularization mechanism at 750 and 800 °C.
described by Seshacharyulu et al. [17] and the schematic illustra- Obviously, a lot of new equiaxed a grains distributed along the
tion was presented in Fig. 14. Here, a brief description is as follows. original grain boundaries indicate that recrystallization is the dom-
Firstly, the plastic deformation leads to the appearance of shear inant globularization mechanism at 850 °C. Furthermore, the a ? b
and generates dislocations of both signs along the planes of shear. phase transformation and recrystallization nucleation and growth
Simultaneously, dislocations of opposite sign are annihilated by will also gradually consume or shorten the original a lamellae,
dynamic recovery duo to the high temperature and only disloca- which also promotes the microstructure globularization. It should
tions of same sign remain along the line of shear. Finally, the b be noted that the coarsening and ripening effect of original a grains
phase penetrates into a lamellae along the shear planes and the cannot be neglected at higher temperature (i.e. 850 °C at here).

Fig. 15. The maps of grain boundaries and the crystal orientation distribution of selected ‘‘short’’ a grains under different deformation conditions: (a) strain of 0.2, strain rate
of 0.01 s1 and temperature of 750 °C, (b) strain of 0.04, strain rate of 0.01 s1 and temperature of 800 °C.
D. He et al. / Materials and Design 46 (2013) 38–48 47

This is why some abnormally thick a grains have been detected at are retained in the recrystallized grains interior (see the magnifica-
850 °C, as shown in Fig. 9b. tion maps in Fig. 7) and the crystal orientations also show a close
relationship (either completely consistent or with a small rotation,
4.3. Recrystallization mechanisms as shown in Fig. 10). Furthermore, the results of the pronounced
high fraction (47–55%) of low angle boundaries (<5°) and relatively
At the temperature of 750 °C, the deformation behavior shows a low fraction (24–33%) of high angle boundaries (>15°) also agree
significant peak and then gradually decreases to a steady state, as well with the basis of CDRX that mentioned above (continuous
shown in Fig. 3a. Generally, this typical hot deformation behavior increase in the misorientation of low angle grain boundaries but
is considered to be caused by a superposition of hardening by dis- limited migration of high angle boundaries).
location storage and softening by (DRX) [29]. Furthermore, a lot of At the temperature of 800 °C, the deformation behavior, micro-
small equiaxed a grains (less than 2 lm in diameter) appeared structure (including grain and subgrain boundary structures) char-
along the original a lamellae, as shown in Figs. 5a and 6a. These acteristics and crystal orientation distribution are basically similar
newly formed small a grains are usually considered as recrystal- to that at 750 °C. However, there are also some differences compar-
lized microstructure. Based on both the deformation behavior ing with the situation at 750 °C. The number and area fractions of
and microstructure characteristics, we can deduce that the recrys- recrystallized grains are significantly increased from 52% and 7% at
tallization occurs in a phase under low strain rate (0.001–0.1 s1) 750 °C to 66% and 12.4%, respectively, as shown in Fig. 16. Further-
and low temperature (750 °C) conditions. more, the distribution of recrystallized grains is more homoge-
However, there are three points worth paying attention to here. neous than that at 750 °C: the recrystallized grains distribute
Firstly, a lot of low and medium angle grain boundaries (<15°) ap- along almost all of the original grains and the ‘‘necklace structures’’
peared in the recrystallized grain interior (see the magnification appear at some regions, as shown in Fig. 6b. On the other hand,
maps in Fig. 7). Secondly, the distribution of recrystallized grain some ‘‘completely new’’ grains (recrystallized grains) without sub-
is relatively heterogeneous: few new grains distribute around the grain boundaries are observed at strain of 0.1 and 0.2, as shown in
original grains which have low Schmid factor for basal slip (e.g. Fig. 8b and c. These results indicate that, beside the CDRX mecha-
0–0.15 for grains marked with ‘‘1’’ in Fig. 6a) and several new nism which is the dominant mechanism at 750 °C, the DDRX mech-
grains appeared nearby the original lamellae with high Schmid fac- anism also appears and plays a complementary role at 800 °C.
tor for basal slip (e.g. 0.35–0.5 for grains marked with ‘‘2’’ in When the deformation temperature increases to 850 °C, the fre-
Fig. 6a). Thirdly, a strongly dependent relationship between the quency of high angle grain boundaries dramatically increases to
crystal orientation distribution of original grains (larger than approximate 60%, as shown in Fig. 13. It is much higher than that
6 lm in diameter) and recrystallized grains (less than 2 lm in at 750 and 800 °C, which is around 30% and 40%, respectively. The
diameter) exists, as seen from the {0 0 0 1} and {1 1 2 0} pole fig- number and area fractions of recrystallized grains steadily in-
ures in Fig. 10. Obviously, all these microstructure and crystal ori- creased to 71% and 16.2%, respectively, as shown in Fig. 16. Obvi-
entation characteristics are different from that formed during a ously, almost all of original a grains are surrounded by
conventional discontinuous dynamic recrystallization (DDRX) recrystallized grains and the necklace structure (i.e. the classic
which usually takes place in cubic metals with low or medium recrystallization structures) appears frequently at the strain of
stacking fault energy [30] but are similar to the characteristics of 0.2, as seen in Fig. 6c. In particular, a lot of ‘‘completely newly
a classic continuous dynamic recrystallization (CDRX) [22]. CDRX formed equiaxed a grains’’, which contain few subgrain boundaries
is accompanied by a continuous increase in the misorientation of within their interior appeared along the original grain boundaries,
low angle grain boundaries with a very limited migration of high as seen in Fig. 9. All these characteristics indicate that the domi-
angle boundaries. Furthermore, because these processes involve nant recrystallization mechanism has been changed to conven-
short-range interactions between dislocations and subgrain tional DDRX at 850 °C from CDRX at 750 or 800 °C. The crystal
boundaries, or between adjacent boundaries, the recrystallized orientations of recrystallized grains showing some extent random
new grains usually present a sharp deformation textures and some distribution (see {1 1 2 0} pole figure in Fig. 12) and a weak corre-
extent similarity in texture components with the retained phase spondence to original grains (see {0 0 0 1} pole figure in Fig.12) also
[22]. validate that the new small recrystallized grains are mainly formed
This CDRX has been frequently observed in hcp metals, e.g. by nucleation and growth.
magnesium alloys [38]. Because the new grain boundaries are In fact, the deformation condition-dependent recrystallization
formed by merging of lower angle boundaries or through accumu- mechanism has also been observed and investigated by other
lation of dislocations into the subgrain boundaries [22], some sub- researchers, e.g. Galiyev et al. pointed out that the mechanism
grain boundaries which are not completely merged or annihilated can change from CDRX in the intermediate temperature range

Fig. 16. Statistical fractions of the recrystallized grains at strain of 0.2. (a) Number fraction versus deformation temperature, and (b) area fraction versus deformation
temperature.
48 D. He et al. / Materials and Design 46 (2013) 38–48

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The author (He Dong) gratefully acknowledges scholarship sup-
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