Intermetallics 19 (2011) 814e819

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Intermetallics
journal homepage: www.elsevier.com/locate/intermet

Creep behaviour of a new air-hardenable intermetallic Tie46Ale8Ta alloy

J. Lapin a, *, T. Pelachová a, M. Dománková b
a
Institute of Materials and Machine Mechanics, Slovak Academy of Sciences, Racianska 75, 831 02 Bratislava, Slovak Republic
b
Faculty of Material Sciences and Technology, Slovak Technical University, Paulínska 16, 917 24 Trnava, Slovak Republic

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

Article history: Creep behaviour of a new cast air-hardenable intermetallic Tie46Ale8Ta (at.%) alloy was investigated.
Received 14 October 2010 Constant load tensile creep tests were performed at initial applied stresses ranging from 200 to 400 MPa
Accepted 15 November 2010 in the temperature range from 973 to 1073 K. The minimum creep rate is found to depend strongly on the
Available online 15 December 2010
applied stress and temperature. The power law stress exponent of the minimum creep rate is n ¼ 5.8 and
the apparent activation energy for creep is calculated to be Qa ¼ (382.9  14.5) kJ/mol. The kinetics of
Keywords:
creep deformation of the specimens tested to a minimum creep rate (creep deformation about 2%) is
A. Titanium aluminides, based on TiAl
suggested to be controlled by non-conservative motion of dislocations in the g(TiAl) matrix. Besides
B. Creep (properties and mechanisms)
D. Microstructure
dislocation mechanisms, deformation twinning contributes significantly to overall measured strains in
the specimens tested to fracture. The initial g(TiAl) þ a2(Ti3Al) microstructure of the creep specimens is
unstable and transforms to the g þ a2 þ s type during creep. The particles of the s phase are preferentially
formed along the grain and lamellar colony boundaries.
Ó 2010 Elsevier Ltd. All rights reserved.

1. Introduction
Investment cast TiAl-based alloys are attractive for various high-
temperature structural applications in the gas turbine and automo-
tive industry. In view of this perspective, there has been a systematic
research and alloy design to improve the room-temperature
ductility, creep resistance, and structural stability by microstructure
control, solid solution alloying and precipitation hardening. These
efforts have resulted in the development of g(TiAl) þ a2(Ti3Al) alloys
containing elements like W, Cr, Mo, Zr, Hf and Nb with a total amount
up to 10 at.% [1e8]. However, the formation of coarse-grained
microstructures during solidification [9] and significant chemical
inhomogeneities of the TiAl-based castings [10] deteriorate the
already low ductility and poor damage tolerance at ambient
temperature. Reducing the grain size in cast components has been
shown to improve significantly room-temperature ductility without
degradation of the creep resistance [11]. Hu et al. [12] showed that
elements such as Nb and Ta have low diffusion coefficients in both
a (Ti-based solid solution with hexagonal crystal structure) and g
phases and favour the massive transformation over the lamellar
formation at low cooling rates. Based on this concept, a new “air-
hardenable” Tie46Ale8Ta (at.%) alloy requiring only air cooling from
single a phase field to reduce the grain size of the cast components
* Corresponding author. Tel.: þ421 2 49268290; fax: þ421 2 44253301.
E-mail address: ummslapi@savba.sk (J. Lapin).
via formation of massive gM(TiAl) was designed [13,14]. This alloy
shows promising castability, mechanical properties and relatively
large processing window to achieve g þ a2 microstructure during
heat treatments [14]. However, potential industrial applications are
conditioned by more complex understanding of its behaviour and
properties at room and high temperatures.
The aim of the present work is to characterise creep behaviour of
a new air-hardenable intermetallic Tie46Ale8Ta (at.%) alloy. This
alloy belongs to the latest 4th generation of TiAl-based alloys, which
has been developed for turbine blade applications within the
European integrated project IMPRESS [15].
2. Experimental procedure
The Tie46Ale8Ta (at.%) alloy was provided in the form of cast
and heat treated cylindrical bars with a diameter of 13 mm and
length of 120 mm. The heat treatments consisted of hot isostatic
pressing (HIP) at an applied pressure of 200 MPa, temperature of
1533 K for 4 h, which was followed by solution annealing at 1633 K
for 1 h and air cooling. The heat treatment was finalized by HIP
ageing at an applied pressure of 150 MPa, temperature of 1523 K for
2 h followed by cooling at a rate of 5 K/min.
Cylindrical creep specimens with a gauge diameter of 6 mm and
gauge length of 30 mm were lathe machined from the as-received
bars. The surface of the specimens was polished to a roughness of
about 0.3 mm. Constant load tensile creep tests were performed at

0966-9795/$ e see front matter Ó 2010 Elsevier Ltd. All rights reserved.
doi:10.1016/j.intermet.2010.11.023
 J. Lapin et al. / Intermetallics 19 (2011) 814e819
Fig. 1. BSEM micrograph showing the typical microstructure of the alloy before creep.
temperatures of 973, 1023, and 1073 K under initial tensile stresses
ranging from 200 to 400 MPa in air. The test temperature was
monitored with two thermocouples touching the specimen gauge
section and held constant within 1 K for each individual test. After
achieving defined creep deformation (or rupture), the creep tests
were interrupted and specimens were furnace cooled to room
temperature under the applied load (or without load in the case of
creep fracture). Specimen displacement was measured using high-
temperature extensometer attached to the ledges of the specimen.
The extensometer was equipped with a linear variable displace-
ment transformer (LVDT). The acquisition of time-elongation data
was accomplished by a computer and data processing was per-
formed by a computer program.
The microstructure evaluation was performed by optical
microscopy (OM), scanning electron microscopy (SEM), back-scat-
tered electron microscopy (BSEM), X-ray diffraction analysis,
energy-dispersive X-ray spectroscopy (EDX) and transmission
electron microscopy (TEM). XRD analysis was carried out using
Bruker D8 DISCOVER diffractometer equipped with X-ray tube with
rotating Cu anode operating at 12 kW. OM and SEM samples were
prepared using standard metallographic techniques and etched in
a solution of 150 ml H2O, 25 ml HNO3 and 10 ml HF. TEM samples
were thinned mechanically to a thickness of about 40 mm and
subsequently electro-polished on a Struers TenuPol-5 twinjet
Fig. 2. TEM bright field micrographs of the alloy before creep: (a) lamellar g þ a2 microstructure with an insert showing selected diffraction pattern, zone axis ½110
(b) g þ a2 microstructure in the vicinity of grain boundaries, zone axis ½1 10g .
815
electro-polisher at 20 V and 233 K. The electropolishing solution
consisted of 65% ethanol, 30% butan-1-ol and 5% perchloric acid.
Volume fraction and size of coexisting phases were determined by
computerised image analysis.
3. Results and discussion
3.1. Microstructure before creep
Figs. 1 and 2 show the typical microstructure of Tie46Ale8Ta
(at.%) alloy before creep. The convoluted type of g þ a2 micro-
structure of the as-received material consists mostly of plate-like
a2 phase which forms small colonies within the g phase. The
lamellae of the a2 and g phases within the colonies maintain
the common Blackburn orientation relationship f111gg kð0001Þa2 ,
as shown in Fig. 2a. A mean length and average volume fraction of
the a2 laths are measured to be 8.5 mm and (29.8  2.3) vol.%,
respectively. Some single-phase a2 and g areas have also been seen
in the microstructure, as shown in Fig. 2b. As shown by Saage et al.
[13], the convoluted microstructure is formed by precipitation of
a and/or a2 phases on four equivalent {111} planes of massively
transformed gM during the second HIP-ing at 1523 K and cooling
from two-phase g þ a field. Fig. 2 indicates that the dislocation
density within the lamellar colonies and single-phase regions is
relatively low and is very similar to that observed by Lapin [16] in
Tie46Ale2We0.5Si (at.%) alloy with a pseudoduplex type of
microstructure.
3.2. Creep
All of the creep curves obtained in this study have the same
basic shape, as shown in Fig. 3. The creep curves exhibit short
primary creep stage that is directly followed by the tertiary creep
(Fig. 3a). Fig. 3b shows variation of the creep rate with the strain.
During the primary creep stage the creep rate decreases with
increasing strain. After reaching a minimum at a strain ranging
from 1.2 to 3.5%, the creep rate increases with increasing strain. No
steady-state creep stage is observed in the tests performed
between 973 and 1073 K with applied stresses ranging from 200
to 400 MPa. The minimum creep rates 3_ min and applied stresses
s were fitted to the power law
3_ min ¼ Asn (1)
where A is a constant and n is the stress exponent. Fig. 4 shows
variation of the minimum creep rate with the applied stress. Using
 k½1120

g a2 ;
816 J. Lapin et al. / Intermetallics 19 (2011) 814e819

Fig. 5. Arrhenius diagram showing dependence of minimum creep rate on inverse

temperature. The applied stresses are indicated in the figure.

where B is a constant, Qa is the apparent activation energy for creep,

R is the universal gas constant and T is the absolute temperature.
Fig. 5 shows the temperature dependence of the minimum creep
rate on the inverse absolute temperature in the form of an Arrhe-
nius diagram. From this figure, the apparent activation energy for
creep calculated for five different applied stresses at three different
temperatures is Qa ¼ (382.9  14.5) kJ/mol. Fig. 6 shows the
minimum creep rate normalised by an exponential term including
the apparent activation energy for creep, absolute temperature and
universal gas constant as a function of the applied stress. It is
obvious that all creep data over the studied temperatures and
Fig. 3. Examples of creep deformation curves at 1023 K: (a) dependence of the creep applied stresses cluster around a straight line. Regression analysis
strain on time; (b) dependence of the creep rate on strain. The applied stresses are of the creep data yields an equation for the minimum creep rate in
indicated in the figures. the form
 
382; 900 J=mol
linear regression analysis of the creep data, the stress exponent n is 3_ min ¼ 2:91  103 s5:8 exp  (3)
RT
determined to vary from 5.7 to 6.0. The correlation coefficients r2 of
these fits are better than 0.96. The correlation coefficient r2 of this fit is equal to 0.98.
The stress-minimum creep rate-temperature data were also The creep characteristics including the stress exponent n and
fitted to the BaileyeNorton power law expression apparent activation energy for creep Qa of the studied alloy can be
  compared with literature data for various TiAl-based alloys where
Qa
3_ min ¼ Bsn exp  (2)
RT

Fig. 6. Minimum creep rate normalised by the apparent activation energy for creep Qa,
Fig. 4. Variation of minimum creep rate with the applied stress. The stress exponents universal gas constant and absolute temperature as a function of the applied stress.
and test temperatures are indicated in the figure. The creep temperatures are indicated in the figure.
 J. Lapin et al. / Intermetallics 19 (2011) 814e819 817

the stress exponent was determined to vary from about 2 at low

stresses to about 10 at high stresses [16e21]. It should be noted that
the stress exponent of n ¼ 5.8  0.3 measured in this study is close
to values of about 5 determined by Parthasarathy et al. [21] from
normalised literature creep data of selected polycrystalline
fully lamellar TiAl-based alloys, or by Lapin [20] for Tie45Al
e2We0.6Sie0.7B (at.%) and Zhang and Deevi [19] for Tie47Ale4
(W,Nb,B) (at.%) alloys. The stress exponent of n ¼ 5.8 obtained in
this work is also close to the experimentally measured and theo-
retically predicted values of about 5 for the creep controlled by
non-conservative motion of dislocations in single-phase alloys [22].
For the activation energy for creep, we can refer to the values
ranging from 230 to 430 kJ/mol reported in the previous studies
[18,20,21,23,24]. The apparent activation energy for creep of
Qa ¼ 382.9 kJ/mol is higher than that of 288e312 kJ/mol and
comparable to 395 kJ/mol determined for self-diffusion of Ti and Al
in Ti3Al, respectively [25e27]. For self-diffusion of Ti and Al in TiAl,
Fig. 7. Comparison of creep behaviour of four TiAl-based turbine blade alloys in the
we can refer to the values of 250e295 kJ/mol and 358 kJ/mol, form of dependence of the applied stress on LarsoneMiller parameter (LMP).
respectively [25,27,28].
For rotating components like turbine blades, creep resistance of
the blade material is of primary importance. Although the the formation of a new s phase is found in both XRD patterns after
maximum overall creep strain allowable for turbine blades creep at 973 K/250 MPa for 3480 h and 973 K/300 MPa for 795 h, as
depends on the engine tolerance, this strain is usually less than 1%. shown in Fig. 8. Crystallographically, the s phase with B82 type
Fig. 7 summarises the dependence of the applied stress on the structure (space group P63/mmc, Pearson symbol hP6) and Ni2In
time to 1% creep deformation in the form of LarsoneMiller symmetry is similar to a ternary hexagonal Ti4Al3Nb phase reported
parameter LMP ¼ T(C þ log t1%), where C is a constant and t1% is the recently by Witusiewicz et al. [29] for Tie46Ale8Nb (at.%) alloy.
time to 1% creep deformation. The LMP is calculated assuming Particles of the s phase are preferentially formed along the grain
a constant of C ¼ 20 and taking the measured time to 1% creep boundaries and lamellar colony boundaries similarly to those
deformation. The studied alloy shows significantly increased time observed by Lapin et al. [30] in long-term aged samples. Fig. 9
to 1% creep deformation when compared to that of ternary indicates that the formation of the s phase is at the expense of the
Tie46Ale8Nb (at.%) alloy [29] at all applied stresses or a2 lathes, which partially transform to the g matrix and s particles
Tie46Ale2We0.5Si (at.%) alloy [20] at higher applied stresses. during creep.
Similar values of LarsoneMiller parameter are calculated for lower
applied stresses of the studied alloy and Tie45Ale2We0.6Sie0.7B
(at.%) alloy [20]. 3.4. Deformation microstructure

3.3. Microstructure stability Deformation in two-phase TiAl-based alloys is well known to

Fig. 8 shows the evolution of X-ray diffraction (XRD) patterns of
the studied alloy during creep. The XRD pattern of the as-received
alloy shows two-phase microstructure composed of the a2 and g,
which is in agreement with the TEM observations and the results
reported recently by Jiang et al. [14]. However, the XRD patterns
reveal that the g þ a2 microstructure is thermodynamically unstable
and transforms to g þ a2 þ s type during creep. The clear evidence of
occur by ordinary dislocations with a Burgers vector b ¼ 1/2h110]
and to a lesser extent by mechanical twinning along 1/6h112] {111}
and by superdislocations with the Burgers vector h110] and 1/2h112]
[18]. The relative contributions of these mechanisms change with
temperature and may sensitively depend on the addition of ternary
or higher alloying elements. Microstructural observations revealed
that the creep of the specimens tested to strains lower than about
3% is dominated by 1/2h110] type of ordinary dislocations, as seen in

Fig. 8. X-ray diffraction patterns of the as-received and crept Tie46Ale8Ta (at.%) alloy. The creep regimes are indicated in the figure.
818 J. Lapin et al. / Intermetallics 19 (2011) 814e819
Fig. 9. TEM bright field micrograph of 486 h creep tested specimen at a temperature of
1023 K and applied stress of 350 MPa, zone axis ½023g .
Fig. 10. TEM bright field micrographs showing the deformation microstructure of the creep specimens tested at: (a) 1023 K/200 MPa to a strain of 2%, zone axis ½415g ; (b) 1023 K/200 MPa
to a strain of 2%, zone axis ½101g ; (c) 1023 K/350 MPa to a strain of 14.7%, zone axis ½121g k½1342a2 .
Fig. 10a. The lamellar interfaces appear to effectively constrain
deformation to individual g lamellae with little evidence for direct
transmission of dislocations under applied creep conditions. The
dislocations in the thicker lamellae tend to be elongated in the
screw orientation and appear to be frequently pinned along their
lengths. The dislocation segments form local cusps along the length
of the dislocations. Such cusps are frequently associated with the
tall jogs on the screw segments of dislocations [31]. The dislocation
segments bowing between the jogs lie on parallel {111} planes and
the jogs themselves lie on a cross slip plane. The deformation
microstructure in the g phase in the vicinity of grain boundaries is
also characterised by pinned ordinary dislocations and formation of
dislocation loops, as seen in Fig. 10b. In addition, the dislocations
form local dislocation network with a square-shape configuration
in the vicinity of some grain boundaries. The dislocation glide at
intermediate and high applied stresses was suggested to be
controlled by non-conservative dragging of such jogs along the
length of screw dislocations [19,31]. As suggested by Appel [32]
using in situ TEM experiments, the jogs move by climb under the
combined action of thermomechanical stresses and osmotic climb
forces arising from the chemical potential of the excess of vacan-
cies. Fig. 10c shows the typical deformation microstructure devel-
oped in the specimens tested to fracture. Besides the dislocation
mechanisms, an intensive formation of deformation twins is
observed in the crept specimens. As suggested by Dlouhý et al. [33],
the meaning of deformation twins is twofold: (i) deformation twins
relax incompatibility stresses during primary creep and (ii) twin-
ning supplies up to the overall strain in advanced stages of creep.
4. Conclusions
The investigation of creep behaviour of a cast intermetallic TiAl-
based alloy with the nominal chemical composition Tie46Ale8Ta
(at.%) suggests the following conclusions:
1. The creep curves show primary creep stage that is directly fol-
lowed by a tertiary creep. The minimum creep rate depends
 J. Lapin et al. / Intermetallics 19 (2011) 814e819
strongly on the applied stress and temperature. The power law
stress exponent n for the minimum creep rate is found to vary
between 5.7 and 6.0 and the apparent activation energy for
creep is calculated to be Qa ¼ (382.9  14.5) kJ/mol.
2. The convoluted g þ a2 microstructure of the creep specimens is
unstable and transforms to the g þ a2 þ s type during creep in
the temperature range 973e1073 K. The particles of the new
s phase with B82 crystal structure are preferentially formed
along grain and lamellar colony boundaries.
3. TEM investigations reveal that the ordinary dislocations in the
g matrix dominate the deformation microstructures at low
creep strains. The dislocations are elongated in the screw
orientation and form local cusps, which are frequently associ-
ated with the jogs on the screw segments of dislocations. Besides
dislocation mechanisms, deformation twinning contributes
significantly to overall measured strain of the specimens tested
to fracture.
4. The kinetics of the creep deformation within the studied
temperature range and applied stresses of the specimens tested
to a minimum creep rate (creep deformation about 2%) is sug-
gested to be controlled by non-conservative motion of disloca-
tions in the g matrix.
Acknowledgments
This work was financially supported by EU Integrated Project
IMPRESS “Intermetallic Materials Processing in Relation to Earth
and Space Solidification” under the contract No. NMP3-CT-2004-
500635 and the Slovak Research and Development Agency under
the contract APVV-0009-07. The authors would like to thank
U. Hecht from ACCESS (Germany) for providing the experimental
material.
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