Intermetallics 66 (2015) 141e148

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

On grain refinement of a g-TiAl alloy using cryo-milling followed by

spark plasma sintering
T. Shanmugasundaram a, b, *, J. Guyon a, b, J.P. Monchoux c, A. Hazotte a, b, E. Bouzy a, b
a
LEM3, CNRS UMR 7239, Universite de Lorraine, Ile du Saulcy, 57045 Metz Cedex 1, France
b
DAMAS (Laboratory of Excellence on Design of Alloy Metals for low mAss Structures), Universit
e de Lorraine, France
c
CEMES, CNRS UPR 8011, Universit
e de Toulouse, 29 rue Jeanne Marvig, BP 94347, 31055 Toulouse Cedex 04, France

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

Article history: A fully dense fine-grained g-TiAl based alloy was fabricated by cryo-milling pre-alloyed powders fol-
Received 23 April 2015 lowed by spark plasma sintering. The consolidation was performed at 1050 or 1200
C. The effect of cryo-
Received in revised form milling on the densification kinetics and final microstructure was studied. Results indicate that cryo-
8 July 2015
milled (8 h) powder is fully densified at a temperature nearly 125
C lower than that of un-milled
Accepted 9 July 2015
Available online 18 July 2015
powder. The microstructure of the alloy fabricated at different temperatures consisted of fine grains of
g-TiAl and a2 (Ti3Al) phases in different volume fractions. The average grain size of cryo-milled powders
compacted at 1050 and 1200
C were determined as 0.6 and 0.9 mm, respectively. It is inferred that the
Keywords:
Titanium aluminides
reduction in crystallite and particle size induced by cryo-milling is the likely reason for such enhance-
Phase transformation ment in densification and grain refinement.
Cryo-milling © 2015 Elsevier Ltd. All rights reserved.
Spark plasma sintering
Microstructure

1. Introduction drastic reduction of consolidation times, resulting in limited grain

Gamma titanium aluminides (g-TiAl) are promising candidate
materials to replace heavy Ni-based superalloys in high tempera-
ture applications due to their attractive properties [1e3]. Currently,
g-TiAl alloys are being used in low pressure turbine aero engine,
exhaust values, and turbocharger for sports and passenger vehicles
[3e6]. However, g-TiAl based alloys are primarily produced via
ingot metallurgy. As a result, they develop a coarse columnar
structure [7]. Indeed, coarse and anisotropic grains generate strong
internal stresses due to deformation incompatibilities [8,9]. On the
other hand, fine-grained TiAl-based alloys are usually produced via
alloying [10,11], thermal [7,12e15], or thermo-mechanical treat-
ments [16e21].
The powder metallurgy route has also been studied as an
alternative method to refine the grain size of metallic and in-
termetallics alloys [22e26]. In this route, atomized pre-alloyed
powders are usually consolidated into bulk by hot pressing
[25,27] or hot isostatic pressing (HIP) [28e30]. More recently, spark
plasma sintering (SPS) has received considerable attention due a
* Corresponding author. LEM3, CNRS UMR 7239, Universite  de Lorraine, Ile du
Saulcy, 57045 Metz Cedex 1, France.
E-mail address: ss.thangaraju@gmail.com (T. Shanmugasundaram).
growth and finer microstructures [31e34]. Consolidation time and
temperature can also be reduced if ball milled powder is used
instead of pre-alloyed atomized powder [31], despite the fact that
ball milling of ductile powders usually results in agglomeration due
to powder sticking [35]. Agglomeration/powder sticking can be
greatly reduced by adjusting the milling intensity, adding process
control agents (PCA's), and/or reducing the milling temperature
(cryo-milling). However, low milling intensity slows alloying and
attrition, while use of PCA's inevitably increases the level of C, H,
and O impurities in the powders because most of the PCAs are
organic compounds (Stearic acid, Toluene, and Methanol) [36,37].
Therefore, ball milling at liquid nitrogen temperature appears to be
a more attractive solution for the sticking problem. In addition,
cryo-milling significantly reduces the milling time and crystallite
size [38e40].
The present work aims to produce fine-grained compacts of g-
TiAl using cryo-milling of pre-alloyed powders followed by spark
plasma sintering. The effect of the initial state of milled powders
(microstructure and morphology of particles) on the densification
kinetics is studied. The microstructural characteristics of the sin-
tered compacts are also presented to characterize the effect of
cryo-milling on the densification and final microstructure
evolution.

http://dx.doi.org/10.1016/j.intermet.2015.07.007
0966-9795/© 2015 Elsevier Ltd. All rights reserved.
142 T. Shanmugasundaram et al. / Intermetallics 66 (2015) 141e148
2. Material and methods
The so-called General Electric (GE) g-TiAl alloy was used in the
present study. Its chemical composition was measured by the
inductively coupled plasma method to be: Tie47.3Ale1.9Cre2.0Nb
(at.%). The powders were produced by Crucible Research (Pitts-
burgh, United States) through gas atomization and were initially
annealed for 1 h at 950
C in an evacuated quartz tube containing a
piece of Ti to minimize the oxidation. This heat treatment was
performed to produce a starting equilibrium (g þ a2) microstruc-
ture to minimize powder sticking and to avoid the phase trans-
formation during SPS. Indeed, ordered intermetallics like the g
phase are generally harder and more brittle than disordered solid
solutions like the a phase. Brittle materials are less prone to powder
sticking than ductile materials during ball milling. Subsequently,
the atomized and annealed (AA) powder was cryo-milled in a
Retsch CryoMill (Haan, Germany) using a vial and balls (10 mm
diameter) made of a hardened steel. The loading and unloading of
the powders was done inside a glove box in argon atmosphere. The
vial and the powder were pre-cooled (15 min) to 190
C at a
milling frequency of 5 Hz, then milled at 20 Hz for different times.
The milling was carried out for up to 8 h with a ball-to-powder ratio
of 10:1. The powders were collected at regular intervals of 2 h for X-
ray diffraction (XRD) and microstructural analysis. XRD measure-
ments were performed using a Co-Ka radiation (1.782 Å) at 40 kV
accelerating voltage and 30 mA current. From the XRD peak pro-
files, instrumental broadening (calibrated using a standard LaB6
peak) and ka2 components were subtracted, and the crystallite size
was estimated using the Scherrer method [41]. The sizes of the AA
and cryo-milled (CM) powder particles were obtained from several
scanning electron micrographs (SEM) using the image analyzing
software Image J [42].
AA powder and powders cryo-milled for 2 and 8 h (CM-2h and
CM-8h, respectively) were consolidated using a Dr Sinter Sumi-
tomo 2080 (Sumitomo Coal Mining Co. Ltd., Japan) spark plasma
sintering (SPS) device. All samples were compacted under a
compression stress of 50 MPa, in a graphite die 8 mm in diameter.
The compacts were heated up to 950
C at a rate of 100
C/min, then
up to the sintering temperature at 25
C/min to avoid overheating.
The temperature was controlled with a pyrometer above 600
C
and the measured temperature corresponds to the external tem-
perature at the surface of the graphite die. The temperatures in the
sample cores were estimated to be 50
C higher for the 8 mm dia.
samples. In the following, temperatures will be referred to as
“control” (measured) or “effective” (estimated, i.e. þ50
C) tem-
peratures. In a first experimental set, the control temperature was
held at 1150
C for 2 min, then both current and pressure were
released at the beginning of the cooling. Dense disks 8 mm in
diameter and about 5 mm in height were produced from about 1 g
of powder. For all powder states (AA, CM-2h and CM-8h), a com-
plementary sample was SPS at lower temperature, in which heating
was stopped at 1000
C. The microstructures of the powders and of
compacted disks were observed using a Zeiss Supra40 (Oberko-
chen, Germany) high resolution scanning electron microscope (HR-
SEM) equipped with a field emission gun. Samples for SEM and
electron backscatter diffraction (EBSD) were prepared by successive
mechanical grinding and polishing followed by a final polishing
with colloidal silica (Struers, Ballerup, Denmark) oxide polishing
suspensions (OPS). Crystallographic analysis was carried out by
EBSD using a Bruker (Billerica, USA) system. EBSD data were
recorded using a 0.07 mm step size and analyzed using HKL Chan-
nel5 software (HKL Technology, Hobro, Denmark). In the EBSD
analysis, the g phase was considered as face centered cubic instead
of tetragonal because the c and a directions were not distinguish-
able [43]. Grain size measurements were obtained using EBSD data.
The average grain size (~2500 grains) was determined by circle
equivalent diameter method. The chemical compositions after SPS
were estimated (5 measurements) using energy dispersive spec-
troscopy (EDS) and the concentration of oxygen was measured (3
samples) using a LECO (St Joseph, USA)TC-436 nitrogen/oxygen
analyzer. The volume fraction of a2 phase was determined using a
point grid method from several low kV (2 kV) SE images (10e15).
Imaging at 2 kV resulted in reduced crystallographic information.
Importantly, both spherical and lath shaped fine precipitates
(~25 nm) were imaged at low kV (2 kV). The volume fraction of the
particles was also determined from the XRD measurements. The
Pearson VII model was used to fit the diffraction peaks and then the
reference intensity ratio (RIR) method was used to estimate the
volume fraction of the a2 phase.
3. Results and discussion
3.1. Characterization of the starting powder
Fig. 1(a) shows the XRD patterns of AA and the as-atomized
powder. The as-atomized powder primarily contains a-Ti phase
(95%) with a small amount of g-TiAl phase (5%). The rapid cooling
from the melting point during atomization suppressed the forma-
tion of the equilibrium g þ a2 structure, resulting in the disordered
metastable a-Ti phase being retained at room temperature. Similar
phase fractions have been observed in the past in an as-atomized
Tie47.3Ale1.9Cre2.0Nb pre-alloyed powder [31]. After annealing
at 950
C, the metastable a-Ti phase transformed to a fully g-TiAl
structure with a small amount (1% ) of a2-Ti3Al phase. An EBSD
map of the annealed powder is shown in Fig. 1(b). The g-phase is in
red and the small amount of a2 phase (blue) is better revealed in the
insert. The high angle boundaries (15
<q < 60
) are marked in black
and twin boundaries (<112> {111}) are marked in white. Grains are
fully recrystallized and equiaxed after annealing. The average g
grain size within the AA powder is about 0.95 mm. About 24% of g
grains contain twin boundaries. The a2-Ti3Al precipitates are nearly
spherical and primarily located at the g grain boundary triple
junctions. The AA powder then further cryo-milled to refine the
particle and crystallite size.1
3.2. Characterization of cryo-milled powders
XRD patterns of the initial AA powder and that of cryo-milled
powders at different milling times are shown in Fig. 2(a). The
presence of superlattice peaks ({001} and {110}) confirms that the
starting AA powder contains substantive amounts of the ordered g
phase. As compared with the sharpness of XRD peaks in the AA
powder, it is seen that milling leads to a progressive broadening of
all peaks, which results in merging of closest peaks, especially those
associated with the tetragonality of the g phase. This broadening is
primarily due to the introduction of deformation defects and to the
refinement of crystallite size during cryo-milling.
The refinement of the crystallite size as a function of cryo-
milling time is shown in Fig. 2(b). In general, the XRD peak
broadening is due to the effect of instrument broadening, crystallite
size, and lattice strain. In the present investigation, due to the peak
overlapping, only the broadening of the {111} reflection was
considered for the crystallite size determination (all of the {111}
planes are equivalent in the L1o structure). The effect from the
instrumental broadening was eliminated using the LaB6 standard
peak, but the effect of lattice strain was not. As a result, the reported
1
In the following, we will use the term “particle” for each powder element, while
the term crystallite will refer to crystalline unit (grain) within powder particles.
 T. Shanmugasundaram et al. / Intermetallics 66 (2015) 141e148 143

Fig. 1. a) XRD patterns of the as atomized and AA powders b) EBSD micrograph of the AA powder (high angle grain boundaries >15
in black and twin boundaries in white lines);
inset band contrast map superimposed with a2-Ti3Al phase in blue. (For interpretation of the references to colour in this figure legend, the reader is referred to the web version of
this article.)

Fig. 2. (a) XRD patterns of AA and cryo-milled powders and (b) crystallite size of the g-TiAl phase as a function of milling time.

crystallite size cannot be considered as an absolute value, but it can
be used for relative comparisons of different milled powders. It is
also worthwhile to note that the size estimated from XRD analysis
was showed to be lower than the size estimated from EBSD/TEM
analysis (when possible). Such discrepancy between XRD and TEM
grain size values has also been reported in another study [44] As
illustrated in Fig. 2(b), the crystallite size of the annealed powder
estimated from XRD was about 230 nm, this size is decreasing with
increasing milling time. The mean crystallite size reaches about
40 nm after 6 h of milling, then does not significantly change with
further milling, indicating that a nearly steady state is achieved at
this stage of milling. The crystallite size of metallic or intermetallics
alloys determined from XRD after ball milling for 10 h is usually in
the range of 30e100 nm [23,25].
SEM micrographs showing the morphology of AA, CM-2h, and
CM-8h powder particles are shown in Fig. 3(aec). The AA powders
are spherical and in the range of 50e150 mm. In general, the initial
stage of ball milling at room temperature is dominated by cold
welding, which results in agglomeration of the powder particles. As
the milling progresses, fracture becomes dominant as the particles
work harden, which results in fragmentation of the powder parti-
cles. In the present case, there is no agglomeration observed during
the initial two hours of milling and the particles rapidly evolve
toward flattened shapes. After 2 h of milling the particle size is in
the range of 25e150 mm, then continuously decreases with
increasing milling time. After 8 h of milling the powder size de-
creases to 2e50 mm, with irregular particle shapes. The CM-8h
powders also contain finer crystallites (Fig. 2(b)) and are expected
to have a larger amounts of residual strain and defects. It is well
known that lattice strain and defect densities increase with milling
time upto a steady state [45].
3.3. Effect of cryo-milling
3.3.1. Densification
The control temperature vs piston displacement curves recor-
ded during SPS densification cycles for AA, CM-2h, and CM-8h
powders are shown in Fig. 4. In these curves, piston displacement
is positive when a sample shrinks (i.e densifies). It can be clearly
seen that most of the consolidation takes place in a restricted
temperature range, which depends on the initial morphology and
microstructure of powder particles. Detectable consolidation starts
at 900
C, 725
C, and 700
C for AA, CM-2h, and CM-8h powders,
respectively. The densification ends at nearly the same temperature
(z1100
C) for the AA and CM-2h powder samples, despite the
earlier start for the CM-2h powder. In CM-8h sample, densification
is nearly finished at a temperature 125
C below the two other
powders (z975
C).
Microscopic observation of samples SPS up to a control tem-
perature of 1150
C shows that all are fully dense. SEM micrographs
of samples consolidated up to the control temperature of 1000
C
are shown in Fig. 5(aec). As expected from Fig. 4, the AA powder
sample still has significant porosity, especially at triple junctions of
particle contact areas (Fig. 5(a)). Some pores are still visible in the
144 T. Shanmugasundaram et al. / Intermetallics 66 (2015) 141e148
Fig. 3. SEM micrographs of the (a) AA (b) CM-2h and (c) CM-8h g-TiAl powder.
Fig. 4. Control temperature vs piston displacement curves recorded during the SPS of
AA, CM-2h and CM-8h powders.
CM-2h sample (Fig. 5(b)), whereas the CM-8h sample appears fully
densified after SPS at the control temperature of 1000
C (effective
temperature equal to 1050
C).
Cryo-milling undoubtedly increases the SPS densification rate
and allows full compaction at lower temperature. Nevertheless, it is
difficult to discriminate between the effects of particle size distri-
bution and shape, and those of microstructure (crystallite size and
defect density). It might be expected that particle shape plays a
major role during the initial stage of the consolidation, which is
governed by plastic deformation at the contact points between
powders that result in local overheating. The occurrence of large
plastic deformation at the particle contact areas has already been
reported [31,46]. This might explain why the detected starting
temperature rapidly decreases at low milling time (2 h). Indeed,
drastic changes in particle shape mostly take place during the early
stages of milling (cf. Fig. 3). During subsequent neck growth and
pore elimination, the influence of initial particle shape is expected
to decrease and microstructure and particle size effects become
dominant. At the intermediate stage, the presence of defects, as
well as the fine crystallite size, enhance the densification. Never-
theless, it should be remembered that some of the stored defects
are probably eliminated during heating due to recovery and
recrystallization [47]. Apparently, the only effect that exists
throughout the process is the particle size. Therefore, it is reason-
able to assume that the particle size plays a major role during the
final stage of sintering. Decreasing the particle size reduces the size
of the micropores. This effect should be important during the pore
elimination process. It is also well known that the smaller the
particle size the higher the inter-particle curvature, which in turns
increases the driving force (interfacial energy) required for neces-
sary neck growth. This can explain why the end of the densification
happens at a lower temperature for the 8 h milled powders than
that for the 2 h milled powders. Such an enhancement in the
densification of ball milled powders has been previously reported
[31].
3.3.2. Microstructural characteristics of SPSed compacts
As this part aims with local observations, temperature values
will refer to effective local temperatures. The chemical composi-
tion of the SPS samples measured by EDS shows that there is no
significant change in the composition from the starting powder
(~Tie47.3Ale2Cre2Nb at.%). More importantly, there is no
contamination of Fe from the ball milling. This is because of the
low milling intensity associated with the cryo-milling (Retsch,
CryoMill). However, noticeable oxygen contamination is detected
 T. Shanmugasundaram et al. / Intermetallics 66 (2015) 141e148
Fig. 5. SEM micrographs of the bulk samples SPS up to a control temperature of 1000
C: (a) AA, (b) CM-2h powder and (c) CM-8h powder.
after SPS of the CM-8h powder. The oxygen content in AA and CM-
8h powder after SPS at 1200
C is 0.15 ± 0.006 and
0.48 ± 0.01 wt.%, respectively. The oxygen content of the CM-8h
powder after SPS at 1050
C is nearly the same
(0.48 ± 0.002 wt.%). Fig. 6 shows EBSD maps of AA and CM-8h
powders compacted by SPS at 1200 or 1050
C. The g-TiAl phase
appears as red and the a2 (Ti3Al) phase as blue. High angle grain
boundaries (>15
misorientation) are marked in black. The
annealing twin boundaries are marked with white lines. When
observed in backscattered electron images, the a2 phase appears
bright grey in a background of the dark g-phase, due to the
chemical contrast (small amounts of orientation contrast are also
observed). Small lath-shaped a2 precipitates (black) are also
observed together with ~ equiaxed (black) a2 precipitates in a
background of the g-phase at low kV (2 kV), shown as the inset in
Fig. 7. The equiaxed a2 precipitates are primarily distributed as a
network along the former particle/g grain boundaries, while the
lath-shaped precipitates appears inside the g grains. Since at low
voltage (2 kV), in secondary electron (SE) mode, the signal
collected with an in-lens detector arises from both SEI and SEII
(induced by backscattered electrons) electrons [48,49], both the
chemical and orientation contrast (a2 phase) can be clearly seen.
Grain sizes and a2 volume fractions of the TiAl based alloy, from
the present and previous studies, are given in Table 1. The volume
fractions of the a2 phase estimated by XRD and grid methods are
nearly the same. The error made on the grid method is about
~0.5%. After SPS at 1200
C, the volume fraction of the a2 phase in
the CM-8h powder is nearly double (20 ± 2%) that of the AA
powder (8 ± 1%). This might be due to the oxygen contamination
because the composition of the other elements is nearly the same
in both the samples. A similar a2 volume fraction (~20e23%) has
also been reported after SPS of ball milled TiAl powder [34].
Nevertheless, the volume fraction of the a2 phase in the CM-8h is
much less after SPS at 1050
C, but the oxygen contamination
(0.48 wt.%) of this sample is nearly the same as in the CM-8h
powder after SPS at 1200
C. This observation suggests that a
145
part of the a2 phase observed after SPS at 1200
C might be
metastable a/a2 phase, which was retained from high tempera-
ture. It is worth noting while 1050
C is below the equilibrium
eutectoid temperature, treatments at 1200
C will result in the
formation of a. The amount of a phase strongly increases with
increasing temperature in the a þ g domain. This can explain the
large amount of a2 phase in the CM-8h sample after SPS at
1200
C.
These results indicate that the microstructure of all the
consolidated samples consists of g-TiAl with different amounts of
a2(Ti3Al). In terms of ductility, the presence of a2 at the former
particle boundaries may not be beneficial. While considering the g
grains, it appears that they are nearly equiaxed and randomly ori-
ented. The average g grain size of the AA powders after SPS at
1200
C is 1.4 mm, whereas the average grain size of the CM-8h
powder SPS at 1050 and 1200
C are 0.6 and 0.9 mm, respectively
(Table 1). As compared to the AA powder, the CM-8h powder after
SPS at 1200
C shows 35% grain refinement. Interestingly, grain
refinement down to 60% (0.6 mm) is observed when the same CM-
8h sample was consolidated at 1050
C. In this sample, the micro-
structure also shows a larger grain size heterogeneity. The grains
near the former-particle surfaces are finer as compared to the
grains in the particle cores. This is due to two reasons. First, the
surface of the powder particles undergoes much more plastic
deformation during cryo-milling, which leads to a higher activation
of recrystallization during SPS. Second, due to grain boundary
hindering by a2 phase, they are higher at the former-particles
surface due to oxygen contamination (Fig. 5).
The observed average grain size in the present study (CM-8h
powder after SPS at 1050
C) is smaller as compared to other re-
ported values (Table 1). The minimum grain size of TiAl based alloys
achieved by thermal treatments [7,14,15] is in the range of
10e65 mm. It is reported that the average grain size of the as-cast
(105 mm) and PM (11 mm) Tie48Ale2Cre2Nb alloys is reduced to
1e7 mm by isothermal forging [20]. For example, an average grain
size of 2e10 mm is observed after SPS of prealloyed atomized TiAl
146 T. Shanmugasundaram et al. / Intermetallics 66 (2015) 141e148

Fig. 6. EBSD micrographs of the bulk samples (a) AA SPS at 1200
C (effective temperature) (b) CM-8h SPS at 1200 and (c) CM-8h SPS 1050
C. g-TiAl is in red and a2-Ti3Al is in blue
colors. High angle grain boundaries (>15
misorientation) are marked in black color. Annealing twin boundaries are marked with white lines, which are defined by a misorientation
of 60
about the <111>. (For interpretation of the references to colour in this figure legend, the reader is referred to the web version of this article.)

Fig. 7. HR-SEM micrograph g-TiAl compacts of (a) AA and (b) CM-8h SPS at 1200
C (c) CM-8h SPS at 1050
C. Insets are low kV images of lath shaped a2 phase.
 T. Shanmugasundaram et al. / Intermetallics 66 (2015) 141e148 147

Table 1
Alloy compositions with their processing history, average grain size, and volume fraction of a2.

Alloy composition (at.%) Processing history Average grain size before Vol. fraction of a2 (Ti3Al) Ref.
and after refinement (mm) balance g-TiAl (%)

Tie47.3Ale1.9Cre2.0Nb Gas atomized and annealed, SPS at 1200
C 1.4 8±1 This work
Tie47.3Ale1.9Cre2.0Nb Gas atomized and annealed þ cryo-milled 0.6 12 ± 1 This work
(8 h) and SPS at 1050
C
Tie47.3Ale1.9Cre2.0Nb Gas atomized and annealed, cryo-milled 0.9 20 ± 2 This work
(8 h) an SPS at 1200
C
Tie48Ale2Cre2Nb As cast þ HIP/deformation þ heat treatment 105/7 e 20
Tie48Ale2Cre2Nb PM þ HIP/deformation þ heat treatment 11/1e3 e 20
Tie48Ale2Cre2Nbe1B As cast/isothermal forging 200/110 e 21
Tie47Ale2Cre2Nb PM þ SPS 2e10 e 33
Tie33Al Prealloyed þ ball-milling (5e30 h) þ SPS 2e4 20e23 34
Tie47Al Ball-milling (36 h) þ SPS at 1000/1100
C 0.5e1.5 e 23
Tie48Ale2Cr As cast þ HIP þ homogenization/cyclic treatment 500/10 e 15
Tie47Ale2Cr As cast/cyclic heat treatment 1000/10e30 e 7
Tie48Ale2Cre2Moe0.25Sie0.3B As cast/cyclic heat treatment 120/30e65 e 14

powder [33]. An average grain size of 0.5e1.5 mm is observed in References

Tie47Al alloy after ball milling for 36 h, followed by SPS at 1100
C
[23]. This shows that grain refinement via powder metallurgy
routes result in smaller grain sizes as compared to other methods.
The present study has shown that cryo-milling followed by SPS is
capable of refining the grain size down to a sub-micron level
(~0.5 mm). The possibility of consolidating TiAl alloys at lower
temperatures owing to cryo-milling has two complementary
beneficial effects. First, it reduces diffusion, thus limiting g grain
growth. Second, it limits the growth of the a2 phase (resulting from
oxygen contamination) by avoiding crossing the eutectoid
temperature.
4. Conclusions
The densification and microstructures of a g-TiAl based alloy
fabricated by cryo-milling of gas atomized powders followed by
spark plasma sintering (SPS) at different temperatures (1200 and
1050
C) have been investigated. Cryo-milling of the atomized (pre-
alloyed) powders shows 100% yield, with a reduction in particle
(2e50 mm) and crystallite size (40 nm). All the samples fully
densified at 1200
C. However, cryo-milling reduces the tempera-
ture required for the densification. The powder cryo-milled for 8 h is
fully densified at lower temperature (1050
C). The microstructure
of the final SPS compacts consists of equiaxed g grains with a2
(6e20% vol. fraction). The oxygen contamination in the AA and CM-
8h sample is 0.15 and 0.48 wt.%, respectively. Both the temperature
and oxygen content play a major role in controlling the a2 volume
fraction. The amount of a2 can be reduced by lowering the consol-
idation temperature. The average grain sizes of the samples
consolidated at 1200
C and 1050
C are 0.9 and 0.6 mm, respectively.
Cryo-milling coupled with SPS is capable of refining the micro-
structure of a g-TiAl alloy to the sub micron level (~0.5 mm). The
grain refinement observed in this study is primarily attributed to the
reduction in crystallite and particle size induced by cryo-milling,
which provide substantial activation energy for the densification.
Acknowledgments
We sincerely thank Dr. M. Thomas (ONERA, France) for
providing the atomized powder and performing their ICP analysis
and Ms. C. Fasel (Dispersive Solids, Technical University Darmstadt,
Germany) for performing the oxygen/nitrogen analysis. The dis-
cussion with Prof. M. Crimp (Michigan State University, USA) is
gratefully acknowledged. TS greatly acknowledges the financial
support from LabEX DAMAS.
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