Journal of Alloys and Compounds 735 (2018) 338e348

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Journal of Alloys and Compounds

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

Effect of continuous cooling on solid phase transformations in

TiAl-based alloy during Jominy end-quench test
J. Lapin*, K. Marek

cesta 9, 845 13 Bratislava, Slovak Republic
Institute of Materials and Machine Mechanics, Slovak Academy of Sciences, Dúbravska

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

Article history: The effect of continuous cooling on solid phase transformations in Ti-47Al-8Ta (at.%) alloy was studied
Received 26 May 2017 using Jominy end-quench test. The microstructure of as-quenched Jominy samples continuously changes
Accepted 7 November 2017 from gM(TiAl) þ a(Ti-based solid solution) through nearly massive gM to lamellar g(TiAl) þ a2(Ti3Al) and
Available online 7 November 2017
gM with increasing distance from the water cooled surface. The cooling curves calculated numerically by
finite element method (FEM) using available material properties deviate from the experimental data. The
Keywords:
application of inverse numerical correlation (INC) method reconciles the calculated cooling curves and
Titanium aluminides
cooling rates with the experimentally measured ones. The highest volume fraction of the massive gM is
TiAl
Phase transformation
achieved at local average cooling rates ranging from 10 to 20  Cs1. While the water and oil cooling from
Microstructure the solid solution annealing temperature leads to numerous short as well as long cracks, the fan and air
Numerical simulation cooling are identified to be suitable for the grain refinement of cast components through formation of
Heat treatment high volume fraction of massive gM grains.
© 2017 Elsevier B.V. All rights reserved.

1. Introduction microstructure such lamellar, Widmanst€ atten lamellar and

Cast TiAl-based alloys are of large interest for high-temperature
structural applications in aerospace, power engineering and auto-
motive industries [1e7]. Their advantage is mainly seen in low
density, high specific yield strength, high specific stiffness, good
oxidation resistance and good creep properties up to high tem-
peratures [8,9]. Various microstructure-properties related studies
suggest that small grains with fine lamellar spacing are optimal for
structural applications [10,11]. There are two main approaches how
to refine coarse grained structure of TiAl-based alloys: (i) alloying
with minor additions, mainly with boron [12e15] and (ii) through
solid phase transformations by appropriate post-solidification heat
treatments [16e23]. According to the importance of diffusion, the
solid phase transformations in TiAl-based alloys can be divided into
two groups: (i) diffusionless massive transformation which in-
volves atom transfers across the interface between the parent a
phase (Ti-based solid solution with hexagonal crystal structure)
and massive gM(TiAl) and (ii) diffusion-related transformations
leading to formation of g(TiAl) þ a2(Ti3Al) two phase
* Corresponding author.
E-mail address: juraj.lapin@savba.sk (J. Lapin).
feathery where two phases have different chemical composition
[16e23]. In many alloys, critical cooling rates to achieve grain
refinement through formation of gM are relatively high which may
result in shape distortion, cracking or even fracture of components
during cooling [21e23]. Low cooling rates required for formation of
gM can be achieved by alloying of TiAl-based alloys with elements
such as Ta and Nb, which have low diffusion coefficient in both g
and a phases and favour the massive transformation over the
lamellar formation [24,25]. Based on this concept, Ti-46Al-8Ta
(at.%) alloy requiring only air cooling from single a phase field to
form massive gM has been designed [26,27]. This alloy shows
promising properties such as good castability, oxidation resistance,
fracture toughness, creep strength, room temperature ductility and
high temperature tensile properties for low pressure turbine (LPT)
blade applications in aircraft engines and stationary gas turbines
[28e35].
The aim of the present work is to study the effect of continuous
cooling from a phase field on solid phase transformations in TiAl-
based alloy with a nominal composition Ti-47Al-8Ta (at.%) using
the Jominy end-quench test. Additional heat treatment experi-
ments are carried out to verify validity of numerical calculations of
heat transfer and demonstrate practical applications of the ach-
ieved results.

https://doi.org/10.1016/j.jallcom.2017.11.076
0925-8388/© 2017 Elsevier B.V. All rights reserved.
 J. Lapin, K. Marek / Journal of Alloys and Compounds 735 (2018) 338e348
2. Methodology and experiment
2.1. Jominy end-quench test
The as-received alloy in the form of cylindrical bar with a
diameter of 90 mm and length of 500 mm was prepared by cold
hearth plasma melting. The alloy was subjected to hot isostatic
pressing (HIP) at a temperature of 1280  C and pressure of 190 MPa
for 4 h to remove cast porosity. The selected HIP temperature cor-
responds to the g þ a phase field of the studied alloy [28]. After the
HIP-ing the bar was cut to smaller pieces with dimensions of
34  34  110 mm3 using wire electrical discharge machining. Two
types of cylindrical samples with a diameter of 25 mm, flange
diameter of 32 mm and length of 107 mm for Jominy end-quench
test were prepared by lathe machining: (i) samples for micro-
structural studies and (ii) samples for experimental measurements
of cooling curves. Before quenching each Jominy sample was
wrapped into tantalum foil with a thickness of 0.1 mm and solution
annealed at a temperature of 1360  C for 1 h in a dynamic argon
atmosphere. The selected solution annealing temperature corre-
sponds to the single a phase field of the studied alloy [28]. After the
solution annealing the sample was removed from the furnace,
quickly transferred to the test fixture and quenched by spraying a
controlled flow of water onto one end, as illustrated in Fig. 1. The
time spent for transferring the sample from the resistance furnace
to the fixture was 2 s. The sample was held for 600 s in the fixture
under controlled cooling conditions. Experimental measurements
of cooling curves were performed with PtRh10-Pt thermocouple
placed into a hole with a diameter of 4 mm drilled along the lon-
gitudinal axis of the Jominy samples at defined distances from the
water cooled surface ranging from 1 to 50 mm. During the water
quenching the temperature acquisition was performed each 0.01 s.
Fig. 1. Schema of Jominy sample with a thermocouple positioned along the axis of the
sample at a distance of 50 mm from the water cooled surface S.
339
2.2. Heat treatments
Heat treatment experiments were carried out to verify validity
and demonstrate practical applications of numerical calculations of
heat transfer and experimental measurements of cooling curves
during the Jominy end-quench tests. The HIP-ed ingot was cut to
smaller bars and lath machined to cylindrical samples with a
diameter of 13 mm and length of 60 mm. Experimental measure-
ments of the cooling curves were carried out with PtRh10-Pt
thermocouple placed into a hole with a diameter of 3 mm and
length of 30 mm drilled along the longitudinal axis of the sample.
The heat treatments consisted of solution annealing at a tempera-
ture of 1360  C for 1 h in dynamic argon atmosphere and cooling to
room temperature using four different cooling mediums: air, fan,
oil and water. During the cooling the temperature acquisition was
performed each 0.01 s.
2.3. Microstructure characterisation
The quenched Jominy samples were cut longitudinally using
wire electrical discharge machining and subjected to metallo-
graphic observations. Metallographic preparation of the samples
consisted of standard grinding using abrasive papers, polishing on
diamond pastes with various grain sizes up to 0.25 mm and etching
in a solution of 100 ml H2O, 6 ml HNO3 and 3 ml HF. Microstructure
evaluation was performed by optical microscopy (OM), X-ray
diffraction (XRD) analysis and backscattered scanning electron
microscopy (BSEM). Chemical composition of the alloy was ana-
lysed by energy-dispersive spectrometry (EDS). Oxygen content
was measured by an elemental analyser using the combustion
technique. The melting of samples for the oxygen measurements
was performed in a graphite crucibles under helium. Oxygen con-
tent was measured in the form of carbon dioxide using infrared
detection. Volume fraction of coexisting structural regions was
measured on digitalized optical micrographs using a computerized
image analyser.
Vickers microhardness measurements were performed at an
applied load of 0.49 N using fully-automatic microindentation
hardness testing system. Average microhardness values were
calculated from 15-20 independent measurements performed at
defined distances from the water cooled surface of the Jominy
samples.
2.4. Density and dilatation measurements
Density and dilatation measurements were carried out for the
purpose of numerical modelling. The density of the studied alloy at
room-temperature was experimentally measured using two fully
dense cylindrical samples with a diameter of 12 mm and length of
140 mm. The density was determined from the weight and volume
of the cylindrical samples.
The dilatation measurements were conducted in argon atmo-
sphere. Cylindrical samples with a diameter of 5 mm and initial
length of 20 mm prepared from the heat treated alloy were sub-
jected to three consequent heating and cooling cycles in a tem-
perature range from 30 to 1380  C at a heating and cooling rates of
3  C/min. A fused quartz bar was used to apply a compression force
of 25 N on the sample during dilatation measurements. The sample
length change was measured by a digital micrometer. The sample
temperature was controlled with an accuracy of ±1  C by a ther-
mocouple touching the sample surface.
2.5. Numerical modelling
Temperature field within the Jominy sample can be described by
340 J. Lapin, K. Marek / Journal of Alloys and Compounds 735 (2018) 338e348
3D Fourier-Kirchhoff heat conduction equation in a cylindrical co-
ordinate system (r, 4, z) for isotropic material and without heat
generation in the form [36,37]
! where Nu is the Nusselt number, L is the characteristic dimension,
vT lðTÞ v2 T 1 vT 1 v2 T v2 T
¼ þ þ 2 þ (1)
vt cp ðTÞrðTÞ v r 2 r vr r v42 v z2
where v2 T=v42 ¼ 0, T is the temperature, t is the time, l(T) is the
thermal conductivity, cp(T) is the specific heat capacity and r(T) is
the density. The thermal conductivity, specific heat capacity and
density are functions of temperature T in Eq. (1). Since a complete
database of thermophysical properties of the studied alloy is not
available, some data published for other TiAl-based alloys are used
in the present work for numerical simulations of the heat transfer
from the Jominy sample during the end-quench test.
For the water jet of surface of the Jominy sample, heat transfer
coefficient varies with sample radius r and surface temperature T.
The heat transfer coefficient HTC(r) depending on the sample radius
r can be estimated as [38,39]:
HTCðrÞ ¼ 5x105 r 5 þ 0:0017r 4  0:0187r 3 þ 0:0571r 2
þ 0:1367r þ 0:4076
Fig. 2 shows dependence of the heat transfer coefficient HTC on
surface temperature (black curve) reported by Le Masson et al. [38]
assuming vaporization, boiling and forced convection on the
surface.
The heat flux q from the water cooled surface of the sample into
surroundings is solved by Newton's law with combined convection
heat transfer in the form [40]
q ¼ hcomb ðTs  Tr Þ
where hcomb is the combined heat transfer coefficient, Ts is the
surface temperature and Tr is the ambient temperature. The com-
bined heat transfer coefficient hcomb is given by the relationship:
hcomb ¼ hconv þ hrad
where hconv is the convection heat transfer coefficient and hrad is
the radiation heat transfer coefficient. Substituting for hconv ¼ lNu/L
and hrad ¼ ε1;2 s0 ðTs2 þ Tr2 ÞðTs þ Tr Þ to Eq. (4), one can obtained
relationship in the form
Fig. 2. Dependence of heat transfer coefficient HTC on surface temperature [38].
lNu  
hcomb ¼ þ ε1;2 s0 Ts2 þ Tr2 ðTs þ Tr Þ (5)
L
ε1,2 is the surface emissivity measured to be 0.94 for the studied
alloy and s0 is the Stefan-Boltzmann constant equal to
(5.67032 ± 0.00071)x108 Wm2K4. One can calculate the con-
vection heat transfer coefficient ranging from 6.3 to 7.1 Wm2K1
which only weakly depends on the temperature. Hence, hconv is
assumed to be constant of 7 Wm2K1 for all numerical calcula-
tions in the present work. Fig. 3 shows temperature dependence of
the calculated combined heat transfer coefficient hcomb (black
curve).
The density, specific heat capacity and thermal conductivity are
used as material properties, which enter into simulation model.
Temperature dependence of density r(T) is calculated according to
relationship in the form
r0 L0
rðTÞ ¼ (6)
L0 þ 3DLðTÞ
where r0 is the density of the studied alloy at room-temperature,
(2)
DL(T) is the temperature dependence of linear elongation of the
sample measured during dilatation test and L0 is the length of the
dilatation specimen at room temperature. The density of the
studied alloy at room temperature is measured to be r0 ¼
(4.960 ± 0.009) g/cm3. Fig. 4 shows dependence of elongation DL on
temperature measured during cooling cycles of the dilatation
experiment (blue curve). In this figure, the temperature depen-
dence of density r (red curve) calculated according to Eq. (6) is used
for the numerical calculations of heat transfer during the Jominy
(3) end-quench test. The second material property applied in the
simulation model is the specific heat capacity cp(T). Fig. 5 shows
experimentally determined dependence of specific heat capacity cp
on temperature (black curve) reported for Ti-46Al-8Nb (at.%) alloy
by Egry et al. [41]. Fig. 6 shows temperature dependence of thermal
conductivity l (black curve) calculated according to relation [42]:
(4)
lðTÞ ¼ aðTÞcp ðTÞrðTÞ (7)
where a(T) is the temperature dependence of the thermal diffu-
sivity. The temperature dependence of the thermal diffusivity was
reported for Ti-46Al-8Nb (at.%) alloy by Egry et al. [41]. The results
Fig. 3. Temperature dependence of combined heat transfer coefficient hcomb.
 J. Lapin, K. Marek / Journal of Alloys and Compounds 735 (2018) 338e348
Fig. 4. Temperature dependence of elongation DL and density r.
Fig. 5. Temperature dependence of specific heat capacity cp [41].
can be well fitted with a third-order polynomial in the form [41]
aðTÞ ¼ 5:36 þ 5:18x103 T  4:30x107 T 2  3:01x109 T 3
where a(T) is in m2s1 and T in  C.
The numerical calculations of the heat transfer were carried out
by finite element method (FEM) using a commercial software
ANSYS at selected distances from the water cooled surface of the
Jominy sample. As a geometrical model of the Jominy sample was
selected a half part of the cylinder. The calculation procedure was
transient and nonlinear with an element size of 0.25 mm and time
step of 0.05 s.
3. Results
3.1. Initial microstructure of Jominy sample
Table 1 shows average chemical composition of the studied alloy
measured by EDS and combustion technique. The studied alloy is
rich in Al (46.9 at.%), Ta (8.4 at.%) and O (860 wt.ppm) compared
with those of 46.0 at.% Al, 8.0 at.% Ta and 490 wt.ppm O reported in
the work of Saage et al. [26]. Fig. 7 shows the typical initial
microstructure of the Jominy samples. Besides the lamellar g þ a2
341
Fig. 6. Temperature dependence of thermal conductivity l.
grains (83.2 vol%), the Jominy samples contain also relatively high
volume fraction of single g grains (16.8 vol%) with an average size of
(35 ± 4) mm, as seen in Fig. 7a and b. The formation of these
equiaxed g grains is connected with the HIP-ing of the studied alloy
at 1280  C in two phase g þ a region. It should be noted that Saage
et al. [26] and Jiang et al. [27] have applied different heat treat-
ments for Ti-46Al-8Ta (at.%) alloy and no equiaxed g grains have
been reported for their samples before Jominy end-quench test.
3.2. Microstructure of Jominy sample after quenching
Fig. 8 shows the microstructure evolution within the Jominy
sample after quenching. It is clear from this figure that the local
microstructure in the sample strongly depends on the distance
from the water cooled surface S. Fig. 9 shows XRD patterns taken at
three distances of l ¼ 2, 20 and 40 mm from the water cooled
surface. In spite of the fact that each XRD pattern indicates four
coexisting phases such as g, massive gM, disordered a and ordered
a2, the individual patterns differ from each other. Increase of the
distance l from 2 to 20 mm leads to an increase of the g/gM
diffraction peaks. Further increase of the distance l to 40 mm results
in a significant increase of ð2021Þa2 diffraction peak. Fig. 10 shows
(8)
the microstructure of the quenched Jominy sample at a distance of
l ¼ 2 mm. The microstructure consists mainly of the retained a
phase and equiaxed near g grains with few coarse a2 laths. The g
grains are usually surrounded by the massive gM, as illustrated in
Fig. 10a and b. Fig. 11 shows the microstructure at a distance of
l ¼ 20 mm. The microstructure consists of the massive gM, equiaxed
near g grains and low volume fraction of lamellar g þ a2 regions
(Fig. 11a and b). Fig. 12 shows the microstructure at a distance of
l ¼ 40 mm. The cooling has no significant effect on the equiaxed
near g grains but leads to the formation of the lamellar g þ a2
microstructure at the expense of the gM (Fig. 12a and b).
Since the quantitative metallographic analysis of the
Table 1
Measured average chemical composition of Jominy samples.
Element
Ti Al Ta O
(at.%) (at.%) (at.%) (wt.ppm)
44.7 ± 0.4 46.9 ± 0.5 8.4 ± 0.2 860 ± 20
342 J. Lapin, K. Marek / Journal of Alloys and Compounds 735 (2018) 338e348

Fig. 7. The typical microstructure of the sample before Jominy end-quench test, OM: (a) regions with duplex type of microstructure; (b) detail showing equiaxed g and lamellar
g þ a2 grains.

Fig. 8. OM micrograph showing longitudinal section of the Jominy sample after quenching, S - water quenched surface.

Fig. 9. X-ray diffraction patterns of the quenched Jominy sample at distances l ¼ 2, 20 and 40 mm.

microstructure of the quenched Jominy samples is performed on
OM micrographs, it is difficult to distinguished between the
retained a phase and fine lamellar g þ a2 microstructure. Therefore,
the quantitative microstructural analysis is supported by Vickers
microhardness measurements. Fig. 13 shows dependence of Vickers
microhardness HVm of various microstructural regions on distance
l. It is clear that the measured HVm values for the retained a phase
are significantly higher than those of the lamellar g þ a2 regions. In
addition, the microhardness values for the gM are clustered well
between those measured for the lamellar g þ a2 regions and near g
grains. The distribution of the HVm values indicates that these
measurements can be used as a supplementary technique for
quantitative metallographic analysis when low magnification and
resolution of OM prevent to identify clearly the specific type of
microstructure.
Fig. 14 shows dependence of volume fractions of the coexisting
microstructural regions on distance l. The main parameter
responsible for the grain refinement of the studied alloy is the
volume fraction of the massive gM formed during the continuous
cooling from the single a phase field. The volume fraction of the gM
increases with increasing distance l and achieves maximum values
ranging from 84 to 94 vol% at the distance l ranging from 8 to
20 mm and decreases at higher distances. A minimum volume
fraction of the gM is achieved at a distance of about 50 mm from the
water cooled surface. The microstructure in this region consists of
the massive gM, equiaxed near g grains and lamellar g þ a2 regions.
At a distance larger than about 60 mm, the heat transfer through
the flange of the Jominy sample to the fixture of the quenching
apparatus leads to an increase of volume fraction of the massive gM
at the expense of the lamellar g þ a2 regions.
 J. Lapin, K. Marek / Journal of Alloys and Compounds 735 (2018) 338e348 343

Fig. 10. The typical microstructure of Jominy sample at a distance of l ¼ 2 mm: (a) OM micrograph; (b) BSEM micrograph.

Fig. 11. The typical microstructure at a distance of l ¼ 20 mm: (a) OM micrograph; (b) BSEM micrograph.

Fig. 12. The typical microstructure of Jominy sample at a distance of l ¼ 40 mm: (a) OM micrograph; (b) BSEM micrograph.

3.3. Effect of cooling rate on microstructure experimentally measured cooling curves according to following
relationship:
Fig. 15 shows experimentally measured cooling curves at
different distances l from the water cooled surface. Fig. 16 shows T1  T2
the results of the numerical calculations of the cooling curves ac- r_c ¼ (9)
t2  t1
cording to the theoretical model, defined boundary conditions and
available material properties at three distances of 2, 20 and 40 mm where T1 is the temperature of 1355  C, T2 is the temperature of
from the water cooled surface in the position of the Jominy sample 700  C, t1 is the cooling time corresponding to T1 and t2 is the
of r ¼ 0 mm (along the longitudinal axis). In the following text we cooling time corresponding to T2. The numerically calculated
will refer to average cooling rates r_c , which are calculated from the cooling curve at the distance of l ¼ 2 mm deviates significantly from
344 J. Lapin, K. Marek / Journal of Alloys and Compounds 735 (2018) 338e348
Fig. 13. Dependence of Vickers microhardness on distance l: G e near g phase, A e
retained a phase, M - massive gM and L e lamellar g þ a2 regions.
Fig. 14. Dependence of volume fraction of coexisting regions on distance l: G e near g
phase, A e retained a phase, M - massive gM and L e lamellar g þ a2 regions.
the experimentally measured one, as seen in Fig. 16a. The average
cooling rate of 240  Cs1 derived from the calculated cooling curve
is significantly higher than that of 75  Cs1 resulting from the
experimentally measured one. Fig. 16b clearly indicates that also
instantaneous cooling rates derived from the calculated cooling
curve achieve a maximum of 278  Cs1 which is significantly higher
than that of 165  Cs1 resulting from the experimental cooling
curve. Fig. 16c shows the calculated cooling curve at the distance of
l ¼ 20 mm, which also deviates significantly from that measured
experimentally. Especially, the experimentally measured cooling
curve clearly indicates a phase transformation which starts at a
temperature of (1237 ± 5)  C. This phase transformation is not re-
flected by the calculated curve. Hence, the difference between the
average cooling rate derived from the calculated cooling curve of 15
 Cs1 and that of 10  Cs1 calculated from the experimental one are
not representative enough due to this phase transformation.
Fig. 16d indicates only one maximum of 16  Cs1 on the cooling rate
curve which was derived from the calculated cooling curve. Two
Fig. 15. Experimentally measured cooling curves at different distances from the water
cooled surface. The distances are indicated in the figure.
maximums of 14  Cs1 and 15  Cs1 are identified on the cooling
rate curve derived from the experimentally measured one. The
phase transformation is also clearly seen on the experimentally
measured cooling curve at the distance of l ¼ 40 mm, as shown in
Fig. 16e. At this distance, the numerically calculated cooling curve
has no evidence of this phase transformation but is clearly indi-
cated by two maximums of 8  Cs1 and 9  Cs1 on the cooling rate
curve derived from the experimentally measured values, as seen in
Fig. 16f.
4. Discussion
4.1. Microstructure of the Jominy samples
As shown by Jiang et al. [27], the massive gM can be formed at a
temperature T0, which is the highest temperature at which a and g
phases of the specific composition have the same free energies.
Based on the phase diagram of Ti-46Al-8Ta (at.%) alloy, T0 was
estimated to be (1220 ± 10) C [27]. This temperature is somehow
lower than that of (1237 ± 5)  C resulting from the cooling curves
shown in Fig. 15.
Figs. 10b, 11b and 12b indicate that the coarse near g grains with
some a2 laths still remain in the quenched Jominy samples. The
origin of these coarse g grains can be found in the applied HIP-ing
of the as-received alloy. In addition, numerous small g grains with
an average size of (7 ± 2) mm are also formed along the grain
boundaries. These small grains are formed during the continuous
cooling of the Jominy samples similarly to those reported by Jiang
et al. [27] for Ti-46Al-8Ta (at.%) alloy. The grain boundary g formed
above T0 reduces the required undercooling, enhances nucleation
and growth and increases temperature range for the formation of
the massive gM [27].
The solid phase transformations observed in the Jominy samples
can be affected also by oxygen content. The oxygen content of
860 wt.ppm in the studied alloy corresponds much better to that
expected in precision cast components than that of about
500 wt.ppm in the laboratory or commercially produced alloys
reported in the previous studies [26e30]. During the continuous
cooling from the a phase field the preferential nucleation sites for
the gM are aea grain boundaries. Huang et al. [43] have observed
that the local oxygen level increases at the grain boundaries during
cooling at slow rates and such higher oxygen content stabilizes the
a phase so that massive transformation can be suppressed locally.
 J. Lapin, K. Marek / Journal of Alloys and Compounds 735 (2018) 338e348 345

Fig. 16. Temperature and cooling rate dependences on time calculated by numerical method, INC method and measured experimentally at various distances l from the water cooled
surface of Jominy sample: (a, b) l ¼ 2 mm, (c, d) l ¼ 20 mm, (e, f) l ¼ 40 mm. Designation of the cooling curves, cooling rate curves and distances l are shown in the figures.

The increase of oxygen content leads to a decrease of volume
fraction of massive gM and increase of volume fraction of retained a
phase in the microstructure [43,44]. On the other hand, the
nucleation and growth of the massive gM is significantly enhanced
within parent a grains when the nucleation at the grain boundaries
is suppressed by stabilization of the a phase with oxygen at low
cooling rates [19,44]. However, this mechanisms of formation gM is
less efficient for the grain refinement than that connected with the
nucleation and growth of gM along the grain boundaries.
4.2. Inverse numerical correlation method
The observed differences between the experimentally measured
cooling curves and those calculated by the numerical method using
FEM and available material properties (Fig. 16) can be minimised by
an inverse numerical correlation (INC) method [39,45]. The INC
method can lead to a more precise computer prediction of the
cooling curves through controlled iterative process consisting of
several fitting steps. In the presents work, each fitting step includes
modification of only one parameter defining boundary conditions
and material properties. Fig. 2 shows the modification of the heat
transfer coefficient HTC (red curve) which is shifted to lower values.
The aim of this modification is to decrease the heat transfer from
the sample at the regions closed to the water cooled surface of the
Jominy sample. However, such modification of the HTC(T) does not
change sufficiently the shape of the cooling curves at the distances
346 J. Lapin, K. Marek / Journal of Alloys and Compounds 735 (2018) 338e348
Fig. 17. Dependence of volume fraction of coexisting regions on average cooling rate. G
e near g phase, A e retained a phase, M - massive gM and L e lamellar g þ a2 regions.
Fig. 18. Experimentally measured cooling curves.
of l ¼ 20 and 40 mm. Therefore, other parameters such as the
combined heat transfer coefficient hcomb, specific heat capacity cp
and thermal conductivity l need to be appropriately modified, as
Fig. 19. OM micrographs showing the typical microstructure after: (a) water cooling and (b) air cooling.
shown in Figs. 3, 5 and 6 (red curves). The application of the INC
method results in new calculated cooling curves shown in Fig. 16a, c
and e (red curves). It is clear that the cooling curves calculated by
the INC method correspond quite well to the experimentally
measured ones (blue curves) including the phase transformations
indicated at a temperature of about 1237  C. Fig. 16b, d and 16f
confirm also a good agreement between the cooling rates derived
from the INC cooling curves and those derived from the experi-
mentally measured data.
4.3. Relationship between Jominy end-quench test and
microstructures formed during heat treatments
The microstructure refinement of the studied alloy based on the
formation of massive gM during continuous cooling should be
applied for sizeable cast components. However, the average cooling
rates measured experimentally and calculated numerically ranging
from 5 to 75  Cs1 in the Jominy samples have more theoretical
than practical meaning, as shown in Fig. 17. Therefore, it is of large
interests to relate these cooling rates to those resulting from the
cooling by different mediums widely used in the technical practice.
Fig. 18 shows experimentally measured cooling curves resulting
from the air, fan, oil and water cooling of the cylindrical specimens
with a diameter of 13 mm and length of 60 mm. The highest
average cooling rate of 48  Cs1 is achieved during the water
cooling. This cooling rate leads to the formation of numerous short
as well as long cracks, as shown in Fig. 19a. The microstructure of
the sample consists of the retained a phase, massive gM and equi-
axed near g grains. The massive gM is preferentially formed at the
grain boundaries and the interfaces between the near g grains and
a matrix. Due to the formation of low volume fraction of the
massive gM (26.9 vol%) and formation of the cracks, the water
cooling is not suitable for the grain refinement of the studied alloy.
Change of the water to the oil cooling significantly decreases the
average cooling rate to 24  Cs1. However, this cooling rate is still
too high and leads to formation of some short and long cracks,
which avoid its practical applications. The microstructure of the oil
cooled sample consists of massive gM (84 vol%), lamellar g þ a2
grains and equiaxed near g grains. The fan cooling of the sample
leads to an average cooling rate of 15  Cs1. This cooling is very
efficient to transform the a phase to gM without the formation of
cracks. The microstructure of the fan cooled sample consists of the
massive gM (94 vol%) and grains with lamellar g þ a2 and near g
microstructure. Due to the formation of high volume fraction of gM
and no tendency to form cracks, the fan cooling is found to be
suitable method for the grain refinement of the studied alloy.
Fig. 19b shows the typical microstructure of the alloy after the air
 J. Lapin, K. Marek / Journal of Alloys and Compounds 735 (2018) 338e348
cooling. The air cooling is characterised by an average cooling rate
of 11  Cs1. The microstructure of the air cooled samples consists of
the gM (92 vol%) and grains with lamellar g þ a2 and near g
microstructure. Since the air cooling is efficient to transfer high
volume fraction of the a phase to massive gM without formation of
cracks or defects, this cooling is industrially fully relevant to refine
the microstructure of cast components from the studied alloy.
The achieved results from the Jominy end-quench and heat
treatment experiments allow to predict a maximum diameter of
cast cylindrical bars which microstructure can be refined reliably
without formation of cracks (see Figs. 14, 17 and 19). Assuming fan
cooling from a solution annealing temperature of 1360  C, a
maximum diameter of cylindrical sample to guarantee the forma-
tion of minimum 83 vol% of gM is 24 mm. This value is in very good
agreements with a value of 25 mm reported by Saage et al. [26] for
Ti-46Al-8Ta (at.%) alloy cooled at a nominal cooling rate of 15  Cs1.
It should be noted that the nominal cooling rates have been
determined using a different methodology [24] than that applied
for the calculation of average cooling rates in the present work.
5. Conclusions
The effect of continuous cooling from a phase field on solid
phase transformations in TiAl-based alloy with the nominal
composition Ti-47Al-8Ta (at.%) has been studied using Jominy end-
quench test. The following conclusions are reached:
1. The local microstructure of the quenched Jominy samples de-
pends on the distance from the water cooled surface. The
microstructure of the quenched samples changes from a þ gM
through nearly gM to lamellar g þ a2 and gM with increasing
distance from the water cooled surface. The highest volume
fractions of the massive gM (higher than 84 vol%) are achieved at
local average cooling rates ranging from 10 to 20  Cs1.
2. The cooling curves calculated by numerical method using FEM
and available material properties deviate significantly from the
experimentally measured data. The application of the INC
method reconciles the calculated cooling curves and cooling
rates with the experimental ones.
3. While the water and oil cooling from the solid solution
annealing temperature leads to numerous short as well as long
cracks, the fan and air cooling are identified to be suitable for the
formation of high volume fraction of the massive gM in the
studied alloy without cracking during the heat treatments.
4. The achieved experimental results from the Jominy end-quench
tests, numerical simulations and applied heat treatment exper-
iments indicate that the fan cooling can be applied for the grain
refinement of cast components with a thickness up to 24 mm.
Acknowledgments
This work was financially supported by the Slovak Research and
Development Agency under the contract APVV-15-0660, the Slovak
Grant Agency for Science under the contract VEGA 2/0125/16, the
Slovak Research and Development Agency under the contract
APVV-0434-10 and the Slovak Academy of Sciences under the
contract of MVTS funding of the project GRADECET. The experi-
mental work was carried out thanks to the infrastructure supported
by the Research and Development Operational Program funded by
the European Regional Development Funds OPVaV-2013/4.2/09-RO
and OPVaV-2013/2.2/09-RO in the frame of the projects: Compe-
tence Center for New Materials, Advanced Technologies and Energy
(ITMS 26240220073), Center for Applied Research of New Materials
and Technology Transfer (ITMS 26240220088) and Center of
Applied Research ALLEGRO (ITMS 26220220198).
347
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