RARE METALS

Vol. 30, Spec. Issue, Mar 2011, p. 462

DOI: 10.1007/s12598-011-0325-2

Microstructure and creep behavior of A 9%W single crystal nickel-based

superalloy
LI Anan, TIAN Sugui, LIANG Fushun, LI Jingjing, WANG Xiaoliang, and ZHANG Te
School of Materials Science and Engineering, Shenyang University of Technology, Shenyang 110870, China
Received 29 September 2010; received in revised form 29 December 2010; accepted 10 January 2011
The Nonferrous Metals Society of China and Springer-Verlag Berlin Heidelberg 2011

Abstract
By means of the measurement of creep curves and microstructure observation, an investigation has been made into the microstructure evolution and creep behaviors of 9%W single crystal nickel-base superalloy. Results show that the alloy displays an obvious sensibility on the applied stress when applied stress is more than 160 MPa at 1040 C. In the ranges of the applied temperatures and stresses, the apparent creep
activation energy is measured to be about 465 kJ/mol. In the initial stage of creep, the cubical phase in the alloy is transformed into the
N-type rafted structure along the direction vertical to the applied stress axis, the deformed mechanism of the alloy during steady state creep is
dislocations climbing over the rafted phase, the dislocation shearing into the rafted phase is thought to be the creep mechanism of the alloy during later stage of creep. After crept up to fracture, the various morphology of the rafted phase is displayed in the different regions of
the sample, the rafted phase vertical to the stress axis displays in the region far from the fracture, but the coarser twisted phase is detected
in the regions near the fracture, which is attributed to the bigger plastic deformation occurred in the region near the fracture.
Keywords: single crystal nickel-base superalloy; element W; microstructure evolution; creep behavior; deformation features

1. Introduction
Single crystal nickel-base superalloys have been widely
used, because they possess high volume fraction of
strengthening phase and good high temperature properties,
for preparing the blade parts of the advanced engine and
combustion turbine [1-3]. The microstructure of the alloy
consists of the cubical phase embedded coherent in the
matrix phase, and the size, morphology and distribution of
the cubical phase are related to the heat treatment process
[4-5]. Adding the refractory elements Re and W can improve the high temperature properties and the creep resistance of superalloys [6-8]. Specially the refractory element
W has the bigger atomic radius and the smaller partitioning
ratio in / phases, and has the higher solubility in the
nickel-base alloy [9-10], so the effect of the solution
strengthening of the alloy increase with the element of W
content. Some literatures reported the creep behavior of single crystal nickel based superalloys [11-12], however, a few
literature reports on the creep behaviors of the W-richer single crystal nickel based superalloy at high temperature.
In the paper, the creep behaviors and the deformation features of the W-richer single crystal nickel based superalloy
are investigated by microstructure observation and creep
Corresponding author: TIAN Sugui

E-mail: tiansugui2003@163.com

curves measuring, and deformation mechanism of the alloy

during creep is briefly discussed.

2. Experimental
The single crystal nickel-base superalloy with [001] orientation has been produced by means of selecting crystal
method in a vacuum directional solidification furnace under
the condition of a high temperature gradient. The nominal
chemical composition of the superalloy is Ni-Cr-Co-AlTa-Mo-9%W (wt,%). The heat treatment regimes of the single crystal nickel based superalloy bars are given as follows:
1280 C 2 h + 1325 C 4 h, A.C + 1080 C 4 h, A.C +
870 C 24 h, A.C.
After the crystal orientation was determined by Laue-back
reflection, the heat treated single crystal bars were machined
into the tensile creep samples along the [001] orientation,
with a cross-section of 4.5 mm 2.5 mm and the gauge
length of 17 mm. The wider surface of the specimen was
parallel to (100) plane. The uniaxial constant load tensile
tests were conducted in the creep testing machine with
GWT504 model. The creep curves of the alloy at the different conditions were measured. The microstructure of the al-

Li A.A. et al., Microstructure and creep behavior of A 9%W single crystal nickel-based superalloy

loy at the different states is observed by using SEM and

TEM. The activation energy and stress exponent of the alloy
during steady state creep are calculated according to the
creep data.

3. Results and analysis

3.1. Creep features of the alloy
The creep curves of the single crystal nickel based superalloy contain 9%W in different conditions are measured as
shown in Fig. 1, indicating that the alloy display the obvious
features of creep three stages, including the initial creep,
steady state creep and accelerated creep stages.
The creep curves of the alloy under the applied stress of
137 MPa at different temperatures are shown in Fig. 1 (a),
this indicates that the bigger initial strain of the alloy occurs
when applying load at high temperature. As the creep goes
on, the dislocation density in alloy increases to decrease the
strain rate up to entering the steady state. The strain rate of
the alloy during steady state creep is measured to be about
0.0144%/h at 1040 C, and the creep lifetime is measured to
be 422 h. As the creep temperature enhances to 1060 C, the
strain rate of the alloy during steady state creep increases to
0.0272%/h, the creep lifetime is measured to be 285 h. In the
further, the creep lifetime of the alloy decreases to 138 h as
the creep temperature enhances to 1072 C.
The creep curves of the alloy under the applied different
stresses at 1040 C are shown in Fig. 1 (b), this indicates that
the strain rate of the alloy during the steady state creep enhances with the applied stress. Under the applied stress of
160 and 180 MPa, the strain rates of the alloy are measured,
respectively, to be 0.0315%/h and 0.0529%/h, the creep lifetimes of the alloy are measured, respectively, to be 200 and
98 h. This indicates that the alloy displays an obvious sensibility on the applied stress when the applied stress is more
than 160 MPa.

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3.2. Constitutive equation and relative parameters

The initial strain of the single crystal nickel based superalloy occurs when applied the tensile stress. As the creep
goes on, the strain rate of the alloy decreases up to entering
the steady state stage, in which the strain rate of the alloy
maintains constant, and the strain rate of the alloy during
steady state creep may be expressed by Dorn creep law
given as follows [11]:
 ss = A An exp(

Q
RT

(1)

where,  ss is the strain rate during the steady state creep, A

being the constant related to material structure, A being
applied stress, n being the apparent stress exponent, R being
the gas constant, T being thermodynamics temperature, Q
being the apparent active energy.
According to the data in Fig. 1, the dependences of the
strain rates of the alloy during steady state creep on the applied temperatures, stresses are shown in Fig. 2. Thereinto,
the relationship between the strain rate and the applied temperatures is shown in Fig. 2 (a), the relationship between the
strain rate and the applied stresses is shown in Fig. 2 (b).
Therefore, the apparent creep activation energy and stress
exponent of the alloy are measured to be Q = 465 kJ/mol
and n = 4.78, respectively. It can be deduced according to
the data that the strain rate of the alloy during steady state
creep is controlled by the climbing of dislocations in the
ranges of the applied temperatures and stresses.
3.3. Influence of heat treatment on microstructure
The microstructures of 9%W superalloy at different
stages of heat treatment, which the samples are eroded by
electrolysis method, are shown in Fig. 3. When the alloy is
solution treated at 1325 C for 4 h, the phase and eutectic
structure in the alloy is completely dissolved, after cooled in
air, the fine phase about 200 nm in size is dispersedly precipitated in the matrix of the alloy, as shown in Fig. 3 (a).

Fig. 1. Creep curves of 9%W single crystal nickel-base superalloy at different conditions: (a) various temperatures under applied
stress of 137 MPa; (b) applied different stresses at 1040 C.

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RARE METALS, Vol. 30, Spec. Issue, Mar 2011

Fig. 2. Relationship between the strain rate and the applied temperatures, stresses during the steady state creep: (a) strain rate &
temperature; (b) strain rate & applied stress.

Fig. 3. Morphology after the alloy heat treated at different

conditions: (a) solution at 1325 C; (b) first aged; (c) full heat
treatment.

After aging treated for 4 h at 1080 C, the fine phase

grows into the cubical configuration about 0.4 - 0.5 m in
size, but the smooth corners is displayed in the cubical
phase, as shown in Fig. 3 (b). After aging treated for 24 h at
870 C, no obvious change in size is detected in the cubical
phase, but the cubical extent of the phase increases, as
shown in Fig. 3 (c). This indicates that no TCP phase is detected in the alloy, and the composition segregation in the
dendrite / interdendrite of the alloy may be reduced [13] to
adjust the size and distribution of the cubical phase during
heat treated at high temperature.

been transformed into the rafted structure along the direction

vertical to the applied stress axis, the thickness of the rafted
phase in the region B is about 0.6 m, as shown in Fig. 4
(c). The morphology of the rafted phase in the region C is
similar to the one in the region B, but the size of the rafted
phase in thickness increases slightly as shown in Fig. 4 (d).
In the further, the twisted configuration of the rafted phase
appear in the region D due to the bigger plastic strain, and
the size of the rafted phase in thickness increases to 0.8 0.9 m, as shown in Fig. 4 (e). The much more coarsening
and twisting of the rafted phase occurs in the region E near
the fracture, so that the size of the phase in thickness increases to about 1 m and the orientation of the rafted phase
have about 45 angle relative to the direction of the applied
stress axis as shown in Fig. 4 (f). It may be considered by
analysis that the coarsening and twisted of the rafted phase
in the region E are attributed to the severe plastic strain.
Under the applied stress of 137 MPa at 1040 C, the microstructure of the alloy crept for different time are shown in
Fig. 5. After crept for 2 h, no fully rafted structure of

3.4. Microstructure evolution of the alloy during creep

After the alloy is crept for 422 h up to fracture under the
applied stress of 137 MPa at 1040 C, the morphologies in
the different regions of the sample are shown in Fig. 4. The
various microstructures are displayed in the different regions
due to the ones supporting the various stress. Therefore, the
deformation extent of the alloy in the different regions may
be analyzed according to the configuration of phase.
The schematic diagram of observing regions in the sample is shown in Fig. 4 (a), no stress is applied in the region A
in which the coarsening of phase occurs only to form the
meshlike structure along the vertical or horizontal directions,
as shown in Fig. 4 (b). But the phase in the region B has

Fig. 4. Morphology of rafts in the different regions after the

alloy crept up to fracture: (a) Schematic diagram of marking
regions in specimen, (b), (c), (d), (e) and (f) being SEM morphologies corresponding to A, B, C, D and E regions of the
specimen, respectively.

Li A.A. et al., Microstructure and creep behavior of A 9%W single crystal nickel-based superalloy

Fig. 5. Morphology of alloy crept for different time under applied stress of 137 MPa at 1040 C: (a) 2 h; (b) crept for 30 h; (c)
crept for 422 h up to fracture.

phase is formed in the alloy, the only several phase is

linked to form the rafted structure along the direction vertical to the stress axis as marked by letter A in Fig. 5 (a). After
crept for 30 h, the creep of the alloy enters the steady state
stage, the phase has been transformed into the rafted
structure along the direction vertical to the stress axis; the
thickness of the rafted phase is about 0.5 m; and the dislocation networks appear in the interfaces between and
phases, as marked by arrow in Fig. 5 (b).
After crept for 422 h up to fracture, the dislocation networks exists still in the interfaces of and phases, and
significant amount of dislocations shear into the rafted
phases as shown in Fig. 5 (c), And the trace of the dislocation displays the feature with 90 folded line as marked by
arrow in Fig. 5 (c), indicating that the cross-slipping of dislocation occurs during creep of the alloy. Thereinto, the direction of the straight-like dislocations is at 45 agree relative to the orientation of the rafted phase, this indicates
that the trace of the dislocations shearing into the rafted
phase is the direction along the biggest shearing stress, and
the rafted phase in the alloy has lost the creep resistance in
the later stage of creep.

4. Discussion
In the initial stage of creep under the applied stress of 137
MPa at 1040 C, the deformation feature of the alloy is that
dislocations move in the matrix channel, no dislocations
shear into the phase. When the creep enters the steady
stage, the deformation mechanism of alloy is that the dislocations climb over the rafted phase and the dislocation
networks appear in the interface of and phases as shown
in Fig. 5 (b). The dislocations networks may relax the lattice
mismatch stress in the interface of / phases [14-15] for
decreasing the interfacial energy to stabilize the microstructure. Meanwhile, the deformed dislocations in the matrix
during creep move to the interfaces to change the original
direction for promoting the dislocation climbing over the
rafted phase, therefore, the interface dislocation plays the

465

coordinating role on the deformed strengthening and recovery softening during creep of the alloy. It can be concluded
that the existence of the interfacial dislocation networks may
delay the dislocations shearing into the rafted phase for
improving the creep resistance of alloy.
In the later period of the creep, some of the dislocation
networks in the interfaces have been damaged because significant amount of dislocations are piled up in the interfaces
for causing the stress concentration as marked by letter A in
Fig. 5 (c), which may result in the dislocation shearing into
the rafted phase for enhancing the strain rate up to the occurrence of the creep fracture.
It is indicated according to the morphology of in different
region of the alloy crept for 422 h up to fracture at 137 MPa/
1040 C that the orientation of the straight-like rafted
phase in the region far from the fracture is vertical to the
stress axis, but the coarsening and twisting extent of the
rafted phase in the region near fracture increase, as shown
in Fig. 4 (f), which indicates that the coarsening and twisting
of the rafted phase increase with the strain of the alloy due
to the reducing the cross-section of the sample and increasing the effective stress. As the creep goes on in the later
stage of creep, significant amount of dislocations are alternately activated along the direction with the maximum
shearing stress for twisting the rafted phase, which results
in the micro-cracks formed in the interfaces of the rafted /
phases, and propagated up to the occurrence of creep fracture. This is thought to be the main reason of occuring the
creep fracture of the alloy.

5. Conclusion
(1) Under the applied stress of 137 MPa at 1040 C, the
9%W single crystal nickel based superalloy displays a lower
strain rate and longer creep lifetime, and displays an obvious
sensibility on the applied stress when the one is more than
160 MPa at 1040 C. In the range of the applied stresses and
temperatures, the apparent creep activation energy of the alloy is measured to be Q = 465 kJ/mol.
(2) In the initial period of creep at 137 MPa / 1040 C, the
cubical phase in the alloy is transformed into the N-type
rafted structure along the direction vertical to the applied
stress axis. As the creep enters the steady stage, the deformation mechanism of the alloy is that the dislocations climb
over the phase, and then the deformation feature of the alloy in the later stage of creep is that dislocations shear into
the rafted phase.
(3) After the alloy is crept up to fracture, the various morphologies of the rafted phase displays in the different regions of the sample. The rafted phase formed along the
direction vertical to the stress axis appears in the region far

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from the fracture, and coarsening and twisting configuration

of the rafted phase are displayed in the region near the
fracture, which is attributed to the severe plastic deformation
of the region.

Acknowledgement
The work was supported by the National Natural Science
Foundation of China (No. 50571070).

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