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Materials Science Forum Online: 2014-04-22
ISSN: 1662-9752, Vol. 788, pp 560-564
doi:10.4028/www.scientific.net/MSF.788.560
© 2014 Trans Tech Publications Ltd, Switzerland

Effect of Long-term Aging on the Microstructures and Stress Rupture

Properties of a Ni-based Single Crystal Superalloy at 980℃
℃

Jianwei Xua, Lili Cuib and Haiwen Wangc

Advanced High Temperature Structural Materials Laboratory, Beijing Institute of Aeronautical
Materials, Beijing 100095, China
a
jianwei-xu@139.com, blili.cui@biam.ac.cn, chaiwen.wang@biam.ac.cn

Key Words: Single Crystal Superalloy, aging time, stress rupture life, γ’ phase, TCP phase.

Abstract. The effect of aging time at 980℃ on the microstructures and mechanic properties for a
single crystal Ni-based superalloy was investigated in this paper. The results showed that γ’ size
distribution portrayed a low growth rate and maintained well cubic during aging for 0~1000h at
980℃. However, γ’ phase was gradually coarsened directionally during the aging for 1000~2500h
at 980℃, indicating that the γ’ phase coarsening was controlled by diffusion during aging for
0~1000h at 980℃. In addition, the γ’ phase coarsening was also susceptible to the interface reaction
during aging for 1000~2500h at 980℃. Furthermore the precipitated phase was analyzed, and the
results showed that only slightly Topologically Close-Packed (TCP) phase was precipitated after
aging for 1500h at 980℃ which indicates that the microstructures of alloy were stable during aging
for up to 1500 hours. At the same time, stress rupture life decreased rapidly for 0~250h, but
basically kept constant value when aged for 250~1500h, then decreased rapidly again aging for
1500~2000h.

Introduction
Ni-base superalloys have been widely used in both aircraft engines and land-based gas turbines
[1]
. At the same time, the efficiency of gas turbine engine has been improved by 1% meaning the
burning temperature must increasing ten temperatures[2]. So the application of single crystal
superalloy can reduce cost and save energy.
As the materials of turbine blades, Ni-based single crystal superalloys undergo for long time at
high temperatures. It is very important that single crystal superalloys keep the microstructure
stability and mechanical property stability after long term exposure at elevated temperatures,
because the blades and vanes of single crystal superalloys work for long time at elevated
temperatures. Some researchers studied the microstructure stability and mechanical property
stability on PWA1484 and SC180[3,5]. The conditions of turbine blade become deteriorate with
increasing need of aerospace engines since the turbine blades bear more complex stress and high
temperature. The morphology, size and distribution of γ’ phase strongly affect on mechanical
properties [3-6]. When the composition and solution treatment have been fixed, aging treatment is
critical to microstructures and properties of alloy, the degree of strengthening is determined by the
volume fraction and size of γ’ phase. Aerospace engine blades are in service at average 980℃ in
long flight. So this article focuses on the changes of the microstructures and properties of a single
crystal superalloy after aging different time at 980℃.

Material and method

The master alloy was melted by vacuum induction melting (VIM), the Ni based single crystal
superalloy bars were solidified by method of selecting crystal with [001] orientation in a directional
solidified vacuum furnace, and the deviations between the [001] crystal orientation of the bars and
the principal axis of stress were maintained within 15 degrees. The compositions of alloy are
Ni-Cr-Co-Mo-Re-W-Al-Ta. The observation surfaces of stress rupture specimens are vertical to
[001]. At first, the test bars were heated treatment which was 1320℃/4h, AC+1130℃/4h, AC +870

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Materials Science Forum Vol. 788 561

℃/32h, AC, then followed by long time aging heat treatment for different time (t=0h, 250h, 500h,
1000h, 1500h, 2000h, 2500h) at 980℃. Test bars after aging long time heat treatment were
machined standard stress rupture specimens as Fig.1. The microstructures of test specimens after
ruptured were observed through field electrical emission microscope (SEM, JSM-6301F).

Fig. 1 Schematic diagram of stress Fig. 2 Effects of different aging time on

rupture specimen stress rupture life at 980℃/250Mpa

Test results and analysis

Effect of aging time on stress rupture life. Alloy after long term aging at 980℃, the stress rupture
tests were performed on conditions of 980℃/250MPa, the results are shown in Fig.1, which
indicates that stress rupture life decreased rapidly for 0~250h, but basically keeps constant value
aging for 250~1500h, then decreased rapidly again with aging for 1500~2000h, as shown in Fig.2.
The reason may be that the rate of γ’ coarsening aging for 0~250h was faster than aging for
250~1500h although γ’ coarsening at low rate aging for 0~1500h, but the Topologically
Close-Packed (TCP) phase was precipitated after aging for 1500h which reducing stress rupture life
decreases rapidly again, as shown in Fig.6.

Fig. 3 Microstructures of different aging time at 980℃, the primary dendrite arm spaces were
(a)0h:0.35µm, (b)500h:0.51µm, (c)1000h:0.55µm, (d)1500h:0.76µm, (e)2000h:0.90µm,
(f) 2500h: 0.92µm.
Effects of aging time on microstructure. The microstructure of alloy after different aging time at
980℃ is shown in Fig.3. It can be observed that the γ’ phase exhibits regular distribution and cubic
shape after standard heat treatment, the γ’ phase had slightly coarsened, but still remaining cubic
when aging for 0~1000h. The γ’ phase obviously coarsened directly, large γ’ phase grew larger and
larger, small γ’ phase continuously eliminated when aging for 1000~2500h. The γ’ phase grew by
joining each other with [100] orientation and exhibited the labyrinth morphology when aging
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562 Structural Materials

exceeding 1000h, as shown in Fig.3(d)~(f)). There are two micro-procedures for γ’ phase
coarsening, one is controlled by diffusion of solute elements of γ’ phase, another is controlled by
boundary reaction where solute elements are dissolved or deposited. A liner-fit curve can be
obtained (Fig.4), which indicates that γ’ phase coarsening is controlled by diffusion for aging of
0~1000h because of the lines very well simulation. However, γ’ phase coarsening is not only
controlled by diffusion but also by boundary reaction for 1000~2500h because of the line’s bad
simulation.

Fig. 4 The coarsening law of γ’ phase

It can be concluded that the alloy microstructures are very stable because of none topologically
close packed (TCP) being observed by scan electrical microscope (SEM) for aging 0~1000h at
980℃. So, this alloy is equal to the second single crystal DD6 superalloy. However, minor needle
pin TCP phase was precipitated with <100> orientation after aging for 1500 hours, long needle TCP
phase which may be probably complex triangle structure µ phase and rich in Re, W was precipitated
after aging for 2000h. In a word, the number of TCP phase was still little and the microstructures of
alloy were still stable after long term aging.

Fig. 5 TCP ( 980℃ /1500h); Fig. 6 TCP (980℃/2000h)

The high volume fraction of γ’ phase which is coherent with γ phase exists in the most of the
single crystal nickel-based superalloys. The shape, size and distribution of γ’ phase significantly
affects on alloy mechanical properties. For example, most of the commercial single crystal
superalloy exhibits excellent stress rupture properties, because γ’ phase has homogeneous
distribution and proper size resulting in huge resistance to dislocations.
Effects of aging time on microstructures near stress rupture fracture. It has been found that the
creep resistance of the nickel base superalloys is affected by the formation of γ’ phase rafts
significantly. The results of the present investigation shows that the shape and size of γ’ phase has
no significant change except cubic decreasing slightly aging for 1000h at 980℃ compared to that of
standard heat treatment (Fig.3), as a result, the mechanical properties of alloy slightly decreased
respectively after aging for 1000h (Fig.2). However, γ’ phase has been coarsened significantly
and exhibits irregular aging for 1500~2500h at 980℃ (Fig.3), as a result, the mechanical properties
deteriorated rapidly respectively (Fig.2). For example, stress rupture life is only 200h after aging
for 2000h. The microstructures 5mm near to stress rupture fracture are shown in Fig.7, it is obvious
that all γ’ phase have been rafted completely and discontinuous (Fig. 7) which decrease resistance
to dislocations.
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Materials Science Forum Vol. 788 563

Fig. 7 Rafting microstructures near 5 mm from fracture surface of stress rupture specimen,(a)aging
for 500h; (b) aging for 1000h; (c) aging for 2000h
After standard heat treatment, γ’ phase exhibits homogenous regular cubic and is coherent with
γ phase. The alloy of crystallographic [100] orientation presents large elastic gradient when loaded
high stress at high temperature after long time aging because of low Young's modulus of [100]
orientation in crystallographic (001) plane. So, it is more higher elastic strain energy of boundary
between γ’ phase and γ phase on (001) plane with [100] orientation comparing to other orientations
[10]
. Under the factors of elastic and boundary energy, γ’ phase grows continuously larger and larger
with [100] orientation. With the increasing stress and time, the dislocation networks appear at the
coherent boundary between γ’ and γ phases. The dislocation networks coordinate coherent
mismatch stress between two phases[8],the compositions of γ’ and γ phase determine the partition of
elements which affects the value of mismatch, and the value of mismatch lastly determines the γ’
phase morphology. The positive or negative of mismatch can be induced from the direction
relationship between rafting and stress axis, for example, N type rafting will be perpendicular to the
stress axis when the alloy's mismatch is positive or negative on the compression or tension
condition respectively (Fig.8). On the contrary, P type rafting will be parallel to stress axis when the
alloy’s mismatch is positive or negative on the tension or compression condition respectively. The
alloy stress rupture properties have been improved with mismatch and γ’ phase cubic increasing .As
shown in Fig.8, the thickness of rafting gradually increases near the crack of fracture, and the cracks
initiate and spread from micro-porosity or boundary of γ/γ’ phase.

Fig.8 Metallurgical structure near the fracture surface of stress rupture for different aging time (980
℃/250Mpa); (a)500h; (b)1000h; (c) 2000h
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564 Structural Materials

Conclusions
(1) γ’ phase gradually grew and maintains well cubic during aging for 0~1000h, directly
coarsening during aging for 1000~2500h at 980℃.
(2) The growth of γ’ phase was controlled by diffusion during aging for 0~1000h, but controlled
by both diffusion and boundary reaction during aging for 1000~2500h at 980℃.
(3) Only minor TCP precipitated during aging for 0~1500h at 980℃ which indicated that the
microstructures of alloy were stable during aging for 0~1500h.
(4) Stress rupture life decreases rapidly for 0~250h, but basically keeping constant value aging
for 250~1500h, then decreases rapidly again aging for 1500~2000h.

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