Physica B 385386 (2006) 523525

Deformation-induced phase development in a cobalt-based superalloy

during monotonic and cyclic deformation
M.L. Benson
a,
, P.K. Liaw
a
, T.A. Saleh
a,b
, H. Choo
a,c
, D.W. Brown
b
, M.R. Daymond
d
,
E.-W. Huang
a
, X.-L. Wang
e
, A.D. Stoica
e
, R.A. Buchanan
a
, D.L. Klarstrom
f
a
Department of Materials Science and Engineering, University of Tennessee, Knoxville, TN 37996, USA
b
Los Alamos Neutron Science Center, Los Alamos National Laboratory, Los Alamos, NM 87545, USA
c
Metals and Ceramics Division, Oak Ridge National Laboratory, Oak Ridge, TN 37831, USA
d
Department of Mechanical and Materials Engineering, Queens Univeristy, Kingston, ON K7L3N6, Canada
e
Spallation Neutron Source, Oak Ridge National Laboratory, Oak Ridge, TN 37831, USA
f
Haynes International, Inc., Kokomo, IN 46904, USA
Abstract
ULTIMET
s
alloy is a metastable face-centered-cubic (FCC) material that undergoes a deformation-induced phase transformation to
a hexagonal-close-packed (HCP) phase. In-situ neutron-diffraction measurements were made at room temperature to study the phase
transformation during monotonic tensile deformation to a total strain of 16% (890 MPa) and also during strain-controlled cyclic
deformation with a total strain range of De 2.5% up to 500 fatigue cycles. The HCP phase developed with increasing strain during the
monotonic-loading experiment, while, during the fatigue deformation, the HCP phase continuously developed with each loading cycle.
Transmission electron microscopy was also performed on monotonically loaded specimens in order to complement the neutron-
diffraction results.
Published by Elsevier B.V.
PACS: 81.30.t; 63.70.th; 25.40.Dn
Keywords: Stress-induced phase transformation; In-situ neutron diffraction; Cobalt-based superalloy
1. Introduction
ULTIMET
s
alloy undergoes a deformation-induced
phase transformation from the metastable FCC structure
to the stable HCP structure [1]. The fatigue behavior of this
material has been extensively characterized by Jiang et al.
[26]. These studies illustrated an unusual temperature
dependency of the fatigue lifetime. Specically, the fatigue
life anomalously increased upon increasing the temperature
from 294 to 873 K, but the lifetime decreased upon
increasing the temperature from 873 to 1173 K. The phase
transformation is also inuenced by the temperature, since
increasing the temperature stabilizes the FCC phase.
Therefore, understanding the phase behavior of ULTI-
MET
s
alloy at different temperatures could provide
insight into the reason for the unique fatigue lifetime
trends of the alloy. In-situ loading neutron-diffraction
experiments were formulated in order to further explore
this issue. In this paper, the results of room-temperature
(RT) in-situ monotonic- and cyclic-loading neutron-dif-
fraction experiments on ULTIMET
s
alloy are presented
to illustrate details of the deformation-induced phase
transformation.
2. Experimental details
ULTIMET
s
alloy is a Co-based superalloy with a
composition of 54Co26Cr9Ni5Mo3Fe2W (weight
percent). The range of grain diameters in the alloy is
50250 mm [2]. The Youngs modulus, 0.2% yield stress,
ARTICLE IN PRESS
www.elsevier.com/locate/physb
0921-4526/$ - see front matter Published by Elsevier B.V.
doi:10.1016/j.physb.2006.05.262

Corresponding author. Tel.: +1 865 974 6356; fax: +865 974 4115.
E-mail address: mbenson2@utk.edu (M.L. Benson).
and ultimate tensile strength at RT are 230 GPa, 524 MPa,
and 1010 MPa, respectively [7].
The in-situ tensile test was performed using the
SMARTS instrument [8]. The tensile specimen was
oriented 451 to the polychromatic incident neutron beam
with the scattering angle xed at 2y 7901 for two
detector banks [8]. The scattering vector is oriented parallel
to the loading direction of the specimen (i.e., the axial data)
and perpendicular to the loading direction of the specimen
(i.e., the transverse data) for the two detector banks.
Neutron-diffraction patterns were measured at 25 points
along the stressstrain curve. Transmission electron micro-
scopy (TEM) was also performed ex situ on two specimens
subjected to tensile stresses of 590 and 840 MPa.
The strain-controlled fatigue was performed using the
ENGIN-X instrument [9] with R 1, where R is the ratio
of the minimum strain (e
min.
) to the maximum strain
(e
max.
). A total strain range of De e
max.
e
min.
2.5% was
applied to the specimen. ENGIN-X employs the same
scattering geometry as SMARTS. Neutron-diffraction
patterns were measured at 10 different fatigue cycles
throughout the fatigue lifetime of 905 cycles. For a given
cycle, six diffraction patterns were measured around the
stressstrain hysteresis loop, as shown in Fig. 1.
3. Results and discussion
An overlay of selected diffraction patterns (axial data)
obtained during the in-situ monotonic-loading experiment
is shown in Fig. 2. The diffraction patterns show that the
material was single-phase FCC in the elastic regime (i.e., up
to 525 MPa). The HCP phase was not resolved by
diffraction until reaching 810 MPa. The intensity of the
1 0

1 1 HCP peak then increased with increasing stress
level.
ARTICLE IN PRESS
800
600
400
M
a
c
r
o
s
c
o
p
i
c

S
t
r
e
s
s

(
M
P
a
)
Macroscopic Strain (%)
200
-200
-400
-600
-800
-2 2 -1 1 0
0
1
2
3
4
5
6
Fig. 1. Diffraction patterns were measured at the points marked on the
stressstrain hysteresis loop.
N
o
r
m
a
l
i
z
e
d

I
n
t
e
n
s
i
t
y
(311)
(220)
(200)
(111)
(1011)
890 MPa
810 MPa
720 MPa
625 MPa
600 MPa
575 MPa
500 MPa
525 MPa
475 MPa
375 MPa
20 MPa
1.4 1.2 1.6 1.8 2.0 2.2
d-spacing (A)
Fig. 2. Overlay of diffraction patterns obtained during in-situ monotonic
loading (axial data).
Fig. 3. TEM micrographs of specimens deformed to (a) 590 and (b)
840 MPa.
M.L. Benson et al. / Physica B 385386 (2006) 523525 524
TEM micrographs of specimens deformed by monotonic
deformation are shown in Fig. 3. At 590 MPa (about
65 MPa above the yield stress) a high stacking-fault density
was apparent, as shown in Fig. 3a. At the relatively high
stress level of 840 MPa, the HCP phase with a needle-type
structure was observed.
The TEM work revealed only stacking faults during the
initial stages of plastic deformation. Therefore, the period
between the onset of yielding and the onset of the
transformation, as discovered in the neutron-diffraction
data, could be characterized by the creation and accumula-
tion of deformation stacking faults.
Fig. 4 shows an overlay of diffraction patterns (axial
data) obtained during strain-controlled cyclic deformation.
Fatigue cycle 12 is reached before the rst HCP diffraction
peak is evident. Following the rst appearance of the peak,
it increased in intensity with increasing fatigue cycles. Two
more HCP diffraction peaks were resolved late in the
fatigue process.
During cyclic loading, the rst fatigue cycle exceeded the
yield stress of the material. However, the maximum stress
attained during cyclic loading was 680 MPa, which is
similar to the stress level considered in Fig. 3a, where no
appreciable HCP phase was observed during the mono-
tonic loading. However, during the low-cycle fatigue, each
cycle supplied a given amount of mechanical energy, which
is associated with the area under the stressstrain hysteresis
loop, to the system [10]. Therefore, the HCP phase
continued to accumulate at the relatively low stress level
during cyclic loading. The initial fatigue cycles could also
be associated with the creation and accumulation of
deformation stacking faults that led to the formation of
the HCP phase.
4. Conclusions
The FCC to HCP deformation-induced phase transfor-
mation in a cobalt-based superalloy was studied by in-situ
loading neutron-diffraction experiments. The HCP during
monotonic and cyclic loading was found to increase as
mechanical energy is supplied to the system, since the
formation of the HCP phase was associated with either (1)
increased area under the stressstrain curve during mono-
tonic loading or (2) repetition of a stressstrain hysteresis
loop during cyclic loading.
Acknowledgments
We thank ISIS Pulsed Neutron and Muon Source and
Los Alamos Neutron Science Center. Financial support
comes from National Science Foundations International
Materials Institutes (DMR-0231320) and Integrative
Graduate Education and Research Training Programs
(DGE-9987548). We also thank the Tennessee Advanced
Materials Laboratory. Additional thanks go to Dr. Yulin
Lu for help with the microscopy.
References
[1] M.L. Benson, T.A. Saleh, P.K. Liaw, H. Choo, D.W. Brown,
M.R. Daymond, X.-L. Wang, A.D. Stoica, R.A. Buchanan,
D.L. Klarstrom, Powder Diffr. 20 (2005) 121.
[2] L. Jiang, C.R. Brooks, P.K. Liaw, J. Dunlap, C.J. Rawn,
R.A. Peascoe, D.L. Klarstrom, Metall. Trans. A35 (2004) 785.
[3] L. Jiang, H. Wang, P.K. Liaw, C.R. Brooks, D.L. Klarstrom, Mech.
Mater. 36 (2004) 73.
[4] L. Jiang, H. Wang, P.K. Liaw, C.R. Brooks, D.L. Klarstrom, Metall.
Trans. A32 (2001) 2279.
[5] L. Jiang, C.R. Brooks, P.K. Liaw, D.L. Klarstrom, C.J. Rawn,
B. Muechen, Mater. Sci. Eng. A316 (2001) 66.
[6] L. Jiang, C.R. Brooks, P.K. Liaw, H. Wnag, C.J. Rawn,
D.L. Klarstrom, Mater. Sci. Eng. A214 (2001) 162.
[7] www.haynesintl.com
[8] M.A.M. Bourke, D.C. Dunand, E. Ustandag, Appl. Phys. A75 (2002)
S1707.
[9] M.W. Johnson, M.R. Daymond, J. Appl. Cryst. 35 (2002) 4957.
[10] G.E. Dieter, Mechanical Metallurgy, third ed., McGraw-Hill,
Boston, 1985, p. 436.
ARTICLE IN PRESS
N
o
r
m
a
l
i
z
e
d

I
n
t
e
n
s
i
t
y
(311)
(1013) (1012)
(220)
(200)
(111)
(1011)
500 cycles
250 cycles
100 cycles
75 cycles
50 cycles
30 cycles
12 cycles
8 cycles
4 cycles
1 cycles
0 cycles
1.4 1.2 1.6 1.8 2.0 2.2
d-spacing (A)
Fig. 4. Overlay of diffraction patterns obtained during in-situ cyclic
loading (axial data).
M.L. Benson et al. / Physica B 385386 (2006) 523525 525