Mechanical behavior of submicron-grained g-TiAl-based

alloys at elevated temperatures

R. Bohn
a,
*, T. Klassen
a
, R. Bormann
a,b
a
Institute for Materials Research, GKSS Research Center Geesthacht, D-21502 Geesthacht, Germany
b
Department of Material Science and Technology, Technical University Hamburg-Harburg, D-21073 Hamburg, Germany
Received 2 March 2001; received in revised form 6 April 2001; accepted 24 April 2001
Abstract
Submicron-grained intermetallic compounds based on g-TiAl were prepared by high-energy milling and hot isostatic pressing. At
temperatures above 500

C, the ow stress is strongly reduced and work-hardening completely disappears. Compression tests per-
formed at temperatures between 500 and 900

C reveal a marked strain rate sensitivity of the ow stress, suggesting superplasticity

to occur. This could be conrmed by tensile straining of Ti45Al2.4Si samples, resulting in elongations of up to 175% at 800

C.
Small silicide particles (d%100 nm) of the type Ti
5
(Si,Al)
3
, embedded in the grain boundaries of the g-TiAl matrix, impede a coar-
sening of the microstructure. However, at strain rates above "
:
10
3
s
1
, these dispersoids are suggested to promote the formation
of voids and to reduce the overall deformability. At 800

C, an apparent activation energy of Q

app
351 kJ/mol can be derived.
Superplastic behavior at 800

C is accomplished by grain boundary sliding accommodated by diusional processes inside the g-TiAl
phase. Thus, the high temperature deformation mode is similar to the mechanisms found for more conventionally grained TiAl
alloys at deformation temperatures 51000

C. # 2001 Elsevier Science Ltd. All rights reserved.

Keywords: A. Nanostructured intermetallics; A. Titanium aluminides, based on TiAl; C. Superplastic forming; C. Mechanical alloying and milling
1. Introduction
Many studies on nano- and submicron-grained mate-
rials have dealt with the mechanical properties at room
temperature, in order to explore the eect of exceptional
microstructural renement on strength and ductility
(e.g. [14]). However, little is known about the mechan-
ical behavior at elevated temperatures 50.5 T
m
, with
T
m
denoting the absolute melting temperature. One
reason may be the low thermal stability of ultrane-
grained materials, giving rise to rapid grain growth
upon increasing the temperature. Consequently, the few
existing studies are mostly concerned with multiphase
metallic systems [58] or ceramics [9], that are less prone
to grain coarsening. Furthermore, specimens with aw-
free microstructures are required, for it was shown that
pores which are a common feature of many powder-
metallurgically processed samples inuence creep
properties via increasing the diusion rates [10]. Creep
tests performed on nanocrystalline NiP and FeBSi
samples result in small stress exponents and lowactivation
energies for creep [6,7], suggesting deformation
mechanisms that are based on grain-boundary-diusion
assisted processes. However, quantitative analysis of the
creep data obtained on nanocrystalline Cu and Pd [8]
demonstrates, that at least for moderate temperatures
up to 0.33 T
m
, the resulting strain rates are much lower
than those according to the equation for Coble creep
[11]. There are also some contradictory results concerning
the grain size dependence of the deformation strain rate.
Whereas Kong et al. show that nanocrystalline samples
deform much faster than their submicron-grained coun-
terparts [5,7], Sanders et al. cannot observe any dierence
between the creep rates of ultrane- or coarse-grained
Cu and Pd samples [8]. In the latter case, a large fraction
of low energy interfaces like twin- and low angle
boundaries was supposed to be responsible for the poor
diusivity and the lack of grain boundary sliding.
Generally, ultrane-grained microstructures with ran-
dom high angle boundaries should promote deformation
at elevated temperatures and lead to easy workable, low
strength materials. This was recently demonstrated by
0966-9795/01/$ - see front matter # 2001 Elsevier Science Ltd. All rights reserved.
PI I : S0966- 9795( 01) 00039- 5
Intermetallics 9 (2001) 559569
www.elsevier.com/locate/intermet
* Corresponding author.
hot working of submicron-grained g-TiAl based com-
pounds [12,13]. Isothermal forging, extrusion as well as
superplastic deformation could be performed at com-
paratively low temperatures or stresses. The purpose of
this study is to elucidate the underlying deformation
mechanisms. Ameyama et al. have shown [14], that the
superplastic behavior of a Ti48Al (in at.%) compound
with a mean grain size of about 1 mm is based on grain
boundary sliding accommodated by lattice diusion
inside the g-TiAl phase. That kind of mechanisms does
not dier from the deformation mode described for
coarser grained material, e.g. by Mishra et al. [15]. In
this study, much ner microstructures are examined,
and the question arises, whether the close meshed net of
grain boundaries contributes to deviations in the defor-
mation behavior. In order to increase the resistance
against grain growth at elevated temperatures, the g-
TiAl matrix of the compounds investigated is reinforced
with a ne dispersion of silicide particles.
2. Experimental
Prealloyed gas-atomized powders of composition Ti
48.9Al and Ti37.5Si as well as pure silicon powders were
mixed in dierent proportions and high-energy milled in
an 8 l attrition mill of Zoz GmbH. Consolidation of the
powders to fully dense compacts was accomplished by hot
isostatic pressing (HIP) at temperatures between 800 and
1000

C. To minimize any contamination of the powders

with atmospheric impurities, milling, transport and sto-
rage of the powders were conducted under vacuum or
controlled gas atmospheres (high purity Ar (99.9999%)
or Ar5 vol.% H
2
). More detailed information about
the powder processing may be taken from Refs. [16,17].
Microstructural investigations were performed using a
Philips CM 200 transmission electron microscope com-
bined with a Link ISIS energy dispersive X-ray analyser.
The average grain size of the consolidated samples was
determined from the micrographs by applying the linear
intercept method. The room temperature microhardness
was measured on metallographically polished samples
under a load of 1 N. Data points represent the average of
40 measurements each. Compression and tensile tests were
carried out on spark-eroded and ground specimens. For
compression testing, cylindrical specimens with a dia-
meter of 4 mm and a length of 8 mm were used. The
Zwick 1478 universal testing machine was equipped with
a three-zone furnace to ensure a constant and uniform
heating of both the specimen and the pistons. In order to
minimize the inuence of oxidation, the compression
tests were run in an atmosphere of owing Ar with a
purity of 99.998%. The compressive strain was recorded
via 3 alumina rods, directly pressed against the specimen
or the upper die, respectively, and connected to a LVDT
outside the heating zone of the furnace. The maximum
deformation detectable was limited to 1 mm, corre-
sponding to a strain of 12.5%. Whereas compression
tests were run with constant velocity, tensile tests on a
Zwick 1484 testing machine were performed using con-
stant strain rates. The corresponding specimens had a
gauge length of 22 mm. Tensile tests could be carried
out only in air.
3. Results
3.1. Microstructure
The intermetallic/ceramic compounds, produced by
high-energy-milling and HIP, are very homogeneous and
consist of equi-axed g-TiAl-grains and x-Ti
5
(Si,Al)
3
-
particles. Depending on the adjusted volume fraction of
the silicide phase, two types of microstructures may be
distinguished.
(a) Intermetallic/ceramic composites with a moderate
silicide content of about 9.6 vol.% (as in Ti45Al2.4Si)
or 13.1 vol.% (as in Ti46Al5Si) reveal a bimodal
grain size distribution, i.e. submicron grains of the
majority phase g-TiAl are surrounded by clearly smaller
particles of the x-Ti
5
(Si,Al)
3
-phase (Fig. 1a). Dierent
HIP-temperatures do not inuence this overall appear-
ance. Volume fractions and arrangement of the phases
involved do not alter, only the phase specic mean grain
sizes vary, but without changing their mutual ratio. An
estimation of the nest grain size achievable under the
applied HIP conditions is given in Ref. [18].
(b) Highly silicide containing compounds like Ti
36Al10Si, with about 30 vol.% of x-Ti
5
(Si,Al)
3
, do not
show any dierence between the mean grain sizes of the
g-TiAl phase and the silicide phase (Fig. 1b). The sili-
cide content is however still low enough to prevent the
formation of a continuous ceramic network, i.e. the
Ti
5
(Si,Al)
3
-grains may be regarded as isolated inclusions
between the g-TiAl crystallites.
Silicon-free binary TiAl-compounds reveal a globular
microstructure of the g phase with small
2
grains pre-
cipitated at the triple points of g grain boundaries [19].
These alloys were included in the study as a submicron-
grained, but silicon-free reference material.
The microstructural data of all samples investigated
were recently published in [4,16] along with their
impurity contents. Considering the multistep powder-
metallurgical processing of the samples, it should be
noted that the amount of contamination by interstitial
atoms like O (%0.3 at.%) and N (%0.1 at.%) is very
low. Nevertheless, the material does not reach the purity
of ingots. As the content of O and N probably exceeds
the solubility limit of the g-TiAl phase, small amounts
of oxides and nitrides should be present within the
microstructure. A more detailed description of the
microstructure is included in Refs. [16,17].
560 R. Bohn et al. / Intermetallics 9 (2001) 559569
3.2. Temperature dependence of yield stress
At low temperatures, submicron-grained alloys based
on g-TiAl are characterized by high values of hardness
and compressive yield strength [20]. As previously
reported [4], this behavior can be explained by the clas-
sical HallPetch relationship, resulting in a 1/
p
d-
dependence of grain size d on yield strength
y
, i.e. dis-
location glide and mechanical twinning as the prevailing
deformation mechanisms are hampered by the ne-
meshed net of grain-boundaries present in submicron-
grained alloys. Consequently, further grain renement
leads to a continued increase of hardness and strength.
In the high temperature range above 500

C, these rela-
tions change completely, i.e. ultrane-grained materials
become very soft. As demonstrated in Fig. 2, there is a
grain size-dependent inversion of yield strength, which
means that the smaller the grain size of the specimen, the
stronger and sharper the drop in yield strength upon
raising the temperature. Silicon-doped g-TiAl-based
compounds with a fraction of up to 32 vol.% Ti
5
(Si,Al)
3
show a similar behavior as the binary TiAl alloys (Fig. 3).
Grain renement causes a reduction of ow stress, sug-
gesting favorable conditions for hot-working of ultra-
ne-grained TiAlSi compounds.
3.3. Strain hardening
Increasing the test temperature leads to a reduction of
strain hardening. As demonstrated in Fig. 4, a binary
TiAl sample with a mean grain size of 670 nm deforms
already at 700

C under constant stress, i.e. the dynamic

sample loading with a given velocity of the crosshead is
comparable to a static loading under a corresponding
constant stress. Thus, the dynamic compression tests are
Fig. 1. TEM micrographs showing the microstructure of TiAlSi compounds in the as-HIPed condition; (a) Ti45Al2.4Si, consolidated at 875

C;
(b) Ti36Al10Si, compacted at 1000

C. Further details are provided in Ref. [16].

Fig. 2. Flow stress after 1.25% plastic compression strain,
1.25
, in
dependence of the deformation temperature for silicon-free alloys;
ML, AM and CF refer to Mechanically Alloyed [19], high energy
Attrition Milled (this work) and Cast/Forged material [21].
Fig. 3. Flow stress
1.25
vs. temperature for Ti46Al5Si and Ti
36Al10Si with a silicide fraction of 13 or 32 vol.%, respectively.
R. Bohn et al. / Intermetallics 9 (2001) 559569 561
formally quite similar to the steady state regime of creep
tests.
1
Specimens with smaller grain sizes show a lack of
strain hardening at still lower temperatures.
3.4. Strain rate dependence of ow stress
Submicron-grained TiAlSi compounds are character-
ized by a marked strain rate sensitivity at temperatures
5500

C. In Fig. 5, the ow stress of dierently ne-

grained specimens of composition Ti45Al2.4Si is
depicted as a function of the applied compression rate
at a temperature of 800

C. The coecient of strain rate

sensitivity, m, that describes the slope of the respective
curves, varies between 0.3 and 0.55. Values of that
magnitude are indicative of superplastic deformation
behavior. However, in order to actually demonstrate the
potential of submicron-grained g-TiAl-based alloys for
superplastic deformation at comparatively low tem-
peratures, tensile tests are required. The corresponding
results are presented in Section 3.6.
The strong strain rate dependence of submicron-
grained TiAlSi compounds has to be kept in mind if the
temperature dependence of the ow stress (Figs. 2 and
3) is interpreted. Especially, from a high ow stress
(under the strain rate conditions applied), it does not
automatically follow that a good creep resistance will be
observed.
At constant stress, decreasing the grain size allows for
higher strain rates to be adjusted in order to reach the
maximum strain rate sensitivity. In the present case, the
bisection of the mean grain size admits about a vefold
increase of the strain rate.
Similar diagrams as in Fig. 5 are attained if the grain
size is kept constant, but the test temperature is chan-
ged. From Fig. 4 in Ref. [13], it is obvious that grain
renement is comparable to a temperature increase with
respect to the deformation behavior. This fact is of great
technological interest, as it allows hot-working of sub-
micron-grained TiAl alloys at reduced temperatures.
3.5. Microstructural stability
Nano- and submicron-grained microstructures are
prone to grain growth due to the large amount of stored
grain boundary enthalpy. Therefore, it has to be inves-
tigated to what extent the mechanical data presented in
the previous sections still refer to the as-HIPed micro-
structures shown in Fig. 1. The grain size of the test spe-
cimens was controlled twice. Firstly, some samples were
annealed at the deformation temperatures of interest and
subsequently cooled down to room temperature. The
dwell time chosen for these heat treatments was 5 h,
which is about 2 h more than the preheating time neces-
sary to adjust a steady temperature prole within the
ceramic pistons of the testing machine. This gives a
reference for the microstructure at the start of the defor-
mation procedure. Secondly, the deformed specimens
were investigated in order to get informations about
microstructural changes occurring upon deformation.
As mentioned before, room temperature hardness and
yield strength of the material are closely related to the
grain size via the Hall-Petch correlation. Therefore,
instead of the time-consuming preparation of TEM
foils, it was sucient to perform hardness measure-
ments in order to get a rst impression of micro-
structural changes. Occasional spot checks carried out
in the TEM revealed that these microstructural changes
were in fact conned to grain growth processes. The
Fig. 4. Compression curves obtained on specimens of composition Ti
48.9Al with a mean grain size of 670 nm.
Fig. 5. Strain rate dependence of ow stress
3.0
(stress after 3.0%
true plastic compression strain) at 800

C for compounds of Ti45Al

2.4Si with dierent mean grain sizes. Fig. 4 represents a completion of
Fig. 5 in Ref. [13].
1
The expression creep test may be somewhat irritating, particu-
larly since deformation rates in the range of 10
4
10
3
s
1
are con-
sidered. However, it should be pointed out that similar deformation
curves as in Fig. 4 are expected by applying a constant stress instead of
a constant crosshead velocity.
562 R. Bohn et al. / Intermetallics 9 (2001) 559569
results of investigations on the microstructural stability
are shown in Figs. 6 and 7. In Fig. 6a, the hardness at
room temperature is plotted against the chosen anneal-
ing temperature. As long as a high hardness level is
retained, grain growth does not occur. The applied HIP-
temperatures are also indicated. As expected, the stabi-
lity of the microstructure at the respective HIP-tem-
perature is enhanced by increasing the amount of the
silicide phase (0!10!13 vol.%). In Fig. 6b, the yield
stresses of the dierent compounds are shown as a
function of the deformation temperature. The three
curves widely overlap. In combination, Fig. 6a and b
show that the marked drop of yield strength occurs
already before the onset of considerable grain growth,
at least in the case of the silicon-doped material.
Accordingly, the decrease of ow stress is rather caused
by a change of the deformation mode than by micro-
structural instabilities of the test specimens. This is an
important result with respect to technological applica-
tions: The low ow stress due to the ne grain size and
the silicide-dispersion-induced stability of the micro-
structure admit favorable hot-working conditions for
the shaping of components.
After compression straining at 800

C, specimens of alloy
type Ti45Al2.4Si do not show any dierence in hardness
between the unstrained or the deformed state, independent
of the strain rate applied (Fig. 7). This allows the conclu-
sion, that the initial microstructure and the respective
mechanical properties did not signicantly change. How-
ever, it also has to be kept in mind that the total compres-
sive strain amounts to only 12.5%, which might be not
enough for the start of strain-induced reactions like
recrystallization. Regarding tensile tests, the preconditions
are somewhat dierent, as discussed in Section 4.
3.6. Tensile straining
Tensile tests at 800

C were performed on the basis of

the mechanical data derived from compression straining
of Ti45Al2.4Si. The experiments were launched to
validate the supposed potential for superplastic deform-
ability and to verify the results obtained by compressive
loading. The results are summarized in Table 1, and may
be described as follows:
1. At strain rates "
:
43:210
3
s
1
elongations
"5175% were reached (Fig. 8). Larger deformations
could not be managed due to the limited length of the
furnace. By increasing the strain rate to "
:
46:4
10
3
s
1
the specimens fail after elongations of 103 or
113%, respectively.
2. The coecients of the strain rate sensitivity are
comparable to those obtained by compression testing.
Increasing the strain rate leads to higher strain rate sen-
sitivities.
3. Simultaneously to an increase of "
:
and m, the frac-
ture strain drops. However, necking of the samples is
not observed.
Fig. 6. (a) Room temperature hardness as a function of annealing
temperature for three g-TiAl based compounds with dierent fractions
of the silicide phase Ti
5
(Si,Al)
3
, according to 0!10!13 vol.%. The
resulting grain growth at temperatures corresponding to the applied
HIP-temperatures is calculated on basis of the HallPetch parameters
given in Ref. [4]. (b) Temperature-dependent ow stress
1.25
of the
same compounds.
Fig. 7. Room temperature hardness, obtained on specimens of com-
position Ti45Al2.4Si after 12.5% compressive deformation at
800

C, in dependence of the applied strain rate. Hardness data refer-

ring to tensile strained specimens B and F is also included (see
Section 3.6 for more details).
R. Bohn et al. / Intermetallics 9 (2001) 559569 563
4. The microstructure has conserved its equi-axed
grain character after deformation (Fig. 9). Contrary to
compression loaded specimens, limited grain growth
occurs. However, within the strain rate range investi-
gated, increasing the deformation rate leads to a reduc-
tion of grain growth.
5. Measurements of the room temperature hardness
were carried out in both the neck and the head region of
deformed specimens. The results are presented in Table 1
and Fig. 7. Whereas the hardness of the specimen heads
did not show any signicant changes in comparison to
the as-HIPed state, the neck regions have become con-
siderably softer, irrespective of the strain rate applied.
As mentioned above, grain growth proved to depend on
the strain rate and thus can not explain the loss of
hardness. Instead, the softening is attributed to the for-
mation of voids, especially in fast strained specimens
(Fig. 10). The accumulation of pores near surface not-
ches indicates that local stress concentrations largely
contribute to cavitation.
4. Discussion
The high temperature mechanical behavior of sub-
micron-grained g-TiAl-based compounds is essentially
characterized by the strongly reduced ow stress. This
property already allowed for rather low consolidation
temperatures during powder processing and implicitly
Table 1
Coecient of strain rate sensitivity, fracture strain, porosity and resulting grain size of Ti45Al2.4Si specimens deformed at dierent strain rates. "
:
1
and "
:
2
are the strain rates applied during the strain rate cycle tests
Fig. 8. Tensile samples of the compound Ti45Al2.4 Si after defor-
mation at 800

C in air. An undeformed specimen is shown for com-

parison.
Fig. 9. TEM micrograph, taken from the neck region of specimen B
after a deformation of 175%. While the grain shape did not change,
slight grain coarsening from 170!248 nm can be observed.
564 R. Bohn et al. / Intermetallics 9 (2001) 559569
contributed to the ne-grained microstructure. In order
to elucidate the mechanisms of high temperature defor-
mation, the stress-strain curves will be further analyzed.
As indicated above, the compression tests can be
treated like static deformation tests, i.e. the compressive
strain rate "
:
which is actually a given parameter
was analysed in dependence of the plateau stress
3:0
arising after an initial plastic deformation of three per-
cent. Generally, "
:
is a function of temperature T, stress
and quite a lot of microstructural parameters S
i
, like
grain size, grain shape, volume fractions and distribu-
tion of phases involved etc.:
"
:
f T; ; S
i
1
In the simplest case, these parameters do not interact.
Assuming that essentially one process is dominating, the
analysis may be based on the equation
"
:
A

E
_ _
n
exp
Q
RT
_ _
2
E denotes the Young modulus, n is the stress expo-
nent and Q refers to the activation energy of the defor-
mation step that is rate-controlling. The inuence of the
microstructural parameters is represented by the pre-
factor A. The slope of the curves shown in Fig. 5 leads
to the respective coecient of the strain rate sensitivity,
m, which is reciprocal to the apparent stress exponent
n
app

dln"
:
dln
_ _
Tconst:

1
m
3
For small stresses, n
app
is about equal to n as long as
the prefactor A does not depend on stress. At larger
stresses, n
app
exceeds n. In advance to the analysis, sev-
eral aspects concerning the microstructural stability
upon high temperature deformation have to be assessed.
1. The mean grain size before and after deformation
was evaluated by hardness measurements. However,
this procedure only oers a selective shot of the truth.
For example, it is possible that a nonvariant grain size is
the result of both grain growth and dynamic recrys-
tallization, that balance each other. This assumption is
supported by studies of Imayev et al. [22] and Koeppe et
al. [23], suggesting that grain renement or grain growth
prevails depending on whether a certain strain rate or
stress level is exceeded or not. The results of the tensile
tests performed within this study tend to support this
view. For the Ti45Al2.4Si compound with a mean
grain size of 170 nm, this neutral strain rate is obviously
larger than 3.210
3
s
1
at 800

C. Thus, it may be
explained why the slowly strained specimen B shows
more intense grain coarsening than specimen F. In
the case of the compression tests, it may be argued that
the strain level attained upon deformation should be too
low to observe similar eects.
2. In strain rate cycle tests performed both in tension
and under compression, the doubling of the strain rate
does not lead to a spontaneous change of ow stress.
Instead, the corresponding stress level is reached rather
gradually, which is indicative of microstructural chan-
ges occurring inside the specimen. Apart from varia-
tions of the grain size, the number and arrangement of
dislocations, twins etc. could account for this behavior.
Consequently, the structure-sensitive prefactor A in Eq.
(2) should not virtually be treated as a constant, and
n
app
should deviate from n. However, the actual dier-
ence must be very small, as strain rate changes from "
:
i
to "
:
i1
(and back) lead to the same plateau stresses that
are reached if the deformation tests are performed with
a strain rate "
:
i1
right from the beginning.
Summarizing, the question of microstructural stability
can be regarded as rather uncritical with respect to the
performed analysis. In this study, n
app
amounts to
values between 1.8 and 3.3. Superplasticity based on
grain boundary sliding requires n=2 [24]. The unchan-
ged grain shape after a tensile strain of 175% provides
strong evidence for grain boundary sliding to play an
important role. In contrast to this, deformation modes
based on diusional ow like Coble [11] or Nabarro
Herring creep [25] are characterized by n 1 and would
lead to an elongation of the crystallites. As this is not
observed, it is concluded that n
app
does not signicantly
overestimate n.
Fig. 10. Evolution of voids in specimen F upon tensile straining at
800

C. The SEM micrograph is taken at the edge of the central neck

region of tensile specimen F. The surface roughness leads to a non-
uniform distribution of voids. A lot of pores have accumulated at the
tip of a notch (arrowed), whereas other regions are essentially free of
voids (encircled).
R. Bohn et al. / Intermetallics 9 (2001) 559569 565
Grain boundary sliding as an essential part of the
superplastic deformation must always be supported by
accommodation processes that prevent the formation of
voids at grain triple junctions. The temperature depen-
dence of deformation can provide further information
about the nature of the assisting mechanism. By plotting
"
:
versus 1/T, the apparent activation energy may be
derived according to
Q
app
R
dln"
:
dln
1
T
_
_
_
_
_
_
const:
4
In Fig. 11, the modulus-compensated strain rate
under compression is plotted against 1/T. The slope of
the curves leads to a value of Q
app
351 kJ/mol, irre-
spective of whether the compounds Ti45Al2.4Si or Ti
36Al10Si are regarded. Obviously, the same mechanisms
are operative in both materials. This is not surprising,
assuming that grain boundary sliding is assisted by pro-
cesses controlled by only the g-TiAl phase. Though
Frommeyer et al. specify an apparent activation energy of
350 kJ/mol also for the deformation of monolythic Ti
5
Si
3
at temperatures between 1000 and 1300

C [27], it seems
unlikely that the hard x-Ti
5
(Si,Al)
3
phase is co-
deformed within a composite containing the softer g-
TiAl phase. This assumption is substantiated by studies
of Wang et al. on powder-metallurgically processed spe-
cimens of composition Ti45Al2.7Si, showing that the
silicide particles are free of dislocations after deformation
at 700

C [28]. The same should be valid with respect to

the still ner silicide grains of this study, especially as
small particles require higher stresses for dislocation
generation and multiplication.
More information about the deformation mode can
be drawn from the grain size dependence of the strain
rate. The microstructure-sensitive parameter A may be
expressed in the form
A / d
p
5
The grain size exponent p results from the slope of a
ln"
:
vs. lnd plot (Fig. 12). At T 800

C and 150
MPa, a grain size exponent of p 2:2 is obtained.
Classifying the experimentally derived parameters,
Q
app
, n
app
and p the deformation mechanism may be
characterized as follows: The apparent activation energy
of 351 kJ/mol is somewhat higher than the reported
activation energy of 250290 kJ/mol for the titanium
self diusion in g-TiAl [29,30]. Nevertheless, it com-
pares well to the published activation energies of com-
paratively coarse-grained g-TiAl alloys (Table 2), that
were deformed at similar or even higher (>1000

C)
temperatures. In connection with a grain size parameter
closer to 2, it is concluded that processes based rather
on volume diusion than on grain boundary diusion
support the grain boundary sliding of submicrocrystal-
line TiAlSi compounds. A corresponding model is sket-
ched in Fig. 13. The diusional ow inside the g-TiAl
grains may be provided by dislocation climb, for exam-
ple. The stress and grain size exponents are very similar
to the values published by Ameyama et al. [14] and
Mishra et al. [15] for the superplastic deformation of g-
TiAl-based alloys with grain sizes of about 1 mm [14] or
20 mm [15], respectively. Thus, the reduction of the
Fig. 11. True compressive strain rate, compensated for the temperature
dependence [26] of the Youngs modulus, as a function of the reciprocal
temperature for compounds of a type Ti45Al2.4Si and Ti36Al10Si.
The analysis was performed at a stress level of 150 MPa.
Fig. 12. True compressive strain rate in dependence of the mean grain
size, demonstrated for samples of composition Ti45Al2.4Si. The
grain size exponent of the deformation was derived for a temperature
of 800

C and a stress level of 150 MPa.

566 R. Bohn et al. / Intermetallics 9 (2001) 559569
mean grain size down to the low submicron range does
not cause a change in the prevailing deformation
mechanism, it rather decreases the lower boundary of
the temperature regime where these mechanisms work.
The results of this study are in some contrast to
recently published work of Imayev et al. [36]. According
to a specied activation energy of 180200 kJ/mol for
the superplastic deformation of submicron-grained
TiAl-based alloys at moderate temperatures of about
750850

C, the authors claim deformation to be

accomplished by grain boundary sliding assisted by dif-
fusion along the grain boundaries. The reason for this
discrepancy cannot be ascertained. However, it should
be noted, that in a corresponding temperature range,
similar specimens as those investigated in [36] require an
activation energy of 335 kJ/mol for grain growth [39],
which rather favours volume instead of grain-boundary
diusion to play a dominant role.
The formation of voids upon superplastic deformation
of g-TiAl alloys is a frequently observed phenomenon
[4042]. Reducing the grain size was shown to be an
appropriate countermeasure [41]. In the present case, a
Table 2
Stress exponents and apparent activation energies obtained from high temperature deformation experiments performed on g-TiAl based alloys
[1415], [19], [3137].
a
and
b
refer to tensile or compression tests, respectively. The alloys marked by * could be superplastically deformed under the
conditions specied
R. Bohn et al. / Intermetallics 9 (2001) 559569 567
lot of pores are visible in the vicinity of surface notches.
Thus it is concluded that stress-induced cavitation plays
an important role. On a submicron scale, hard silicide
particles are supposed to be responsible for the occurrence
of local stress concentrations leading to the formation of
voids all over the neck of the sample. This may be illu-
strated by replacing grain 3 of Fig. 13 by a silicide particle
impermeable for dislocations. In general, the grain triple
points can be identied as preferential nucleation sites for
the formation of cracks [43]. According to Stroh [44],
cracks may be initiated if the shear stress exceeds a
critical value of

c

12G
L
6
with denoting the surface energy and L representing
the length of the glide area. From Eq. (6) it is obvious
that grain renement allows for higher critical stresses.
On the other hand, a lot of triple points are occupied by
silicide particles that could reduce the surface energy
and thus balance out the positive inuence of a small
grain size. In this respect, an even ner distribution of
smaller silicides might be useful.
5. Summary and conclusions
1. Multiphase g-TiAl-based compounds with a very
ne-grained microstructure were produced by high
energy milling and hot isostatic pressing. The grain size
of the g-TiAl matrix amounts to about 160480 nm,
whereas the size of precipitated x-Ti
5
(Si,Al)
3
particles
varies between 80 and 190, depending on the HIP con-
ditions.
2. At temperatures above 500

C, these alloys become

very soft. The smaller the grain size, the stronger the drop
of ow stress. Deformation occurs without any strain
hardening.
3. During deformation at high temperatures, the nely
dispersed silicide particles prevent grain growth as long as
the HIP temperature is not exceeded.
4. The ow stress is rather sensitive to the applied
strain rate. Superplasticity becomes feasible at 800

C,
allowing elongations 5175%. The apparent activation
energy of deformation was assessed to be Q
app
351 kJ/
mol. In connection with a stress exponent around n 2
and a grain size exponent of p 2:2, it is concluded that
the superplastic deformation is accomplished by grain
boundary sliding accommodated by diusional pro-
cesses inside the g-TiAl grains. Such a mechanism does
not dier from the deformation modes described for con-
ventionally grained materials deformed at temperatures
51000

C.
5. The silicide phase is not directly involved in the
process of deformation. In particular, Ti36Al10Si
compounds with about 32 vol.% of the silicide phase
reveal the same activation energy as alloys of composi-
tion Ti45Al2.4 Si with only 9.6 vol.% Ti
5
(Si,Al)
3
. In
both cases only the g-TiAl phase seems to contribute to
the overall deformation. However, changes are expected
if the silicide content is high enough to form a con-
tinuous network within the g-phase.
6. Increasing the tensile strain rate supports the for-
mation of stress induced voids that reduce the overall
deformability. The silicide particles are supposed to
promote cavitation.
Acknowledgements
This work has been supported by the Deutsche For-
schungsgemeinschaft (German Science Foundation)
within the scope of Sonderforschungsbereich 371.
Thanks are due to Dr. R. Gerling for providing the
powders for high energy milling. The experimental help
of U. Lorenz and R. Behn is gratefully acknowledged.
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