Effects of Long-Term Thermal Exposure on the Microstructure

and Properties of a Cast Ni-Base Superalloy

X.Z. QIN, J.T. GUO, C. YUAN, C.L. CHEN, and H.Q. YE

Microstructural stability and microstructure-property relationship during long-term thermal

exposure in K452 alloy (a new Ni-base cast superalloy with ~21 pct Cr, 11 pct Co, 3.5 pct W,
2.5 pct Al, 3.5 pct Ti, and others) are investigated. It is found that exposure temperature and time
have significant effects on the microstructure and properties of the alloy. During exposure, the
microstructure is degraded by c¢ coarsening, MC carbide (M mainly represents Ti, W, and Nb)
degeneration, precipitation and evolution of grain interior (GI) M23C6 carbide, evolution of
grain boundary (GB) microstructure, and precipitation of g phase. Among them, the c¢ coars-
ening is the leading reason for the decrease of strength of the alloy. The GI M23C6 and the g phase
have negligible influence on the properties due to their relatively small populations. Blocky,
closely spaced GB M23C6 particles engulfed in c¢ increase the stress-rupture life, whereas the
formation of a continuous GB M23C6 chain has an opposite effect. A life peak occurs when the
M23C6/c¢ structure at the GBs is in an optimal form. The degenerated MC is the preferred
initiation site of microcracks. Its presence at the GBs promotes the onset of intergranular frac-
ture, and leads to the decrease in mechanical properties.

DOI: 10.1007/s11661-007-9381-5

The Minerals, Metals & Materials Society and ASM International 2007

I. INTRODUCTION tance and service life. In this article, the microstructural

evolution during long-term thermal exposure in the
THE K452 alloy is a newly developed high Cr K452 alloy is examined in detail, and the microstruc-
content cast Ni-base superalloy for advanced gas ture-property relationships are explored carefully.
turbine vane applications in marine and industrial fields.
It performs well under laboratory conditions with good
fatigue resistance, hot-corrosion resistance, and tensile-
and stress-rupture properties, in addition to being II. EXPERIMENTAL PROCEDURE
completely oxidation resistant up to 900 C.[1] K452 has the composition (wt pct) of 0.105C, 20.9Cr,
Compared to aircraft engines, gas turbines for indus- 11.15Co, 3.5W, 0.6Mo, 0.25Nb, 2.5Al, 3.5Ti, 0.04Zr,
trial applications, which are exposed to corrosive 0.015B, and rest Ni. Specimens were subjected to a
environment for prolonged periods of time, have more homogenization for 4 hours at 1170 C followed by
stringent requirements for the hot-end superalloy com- furnace cooling to 900 C and then air cooling to room
ponents to accommodate for their formidable operating temperature; subsequently, two annealing treatments
conditions. Accordingly, for Ni-base superalloys such as (4 hours at 1050 C and 16 hours at 850 C), producing
K452, microstructural stability is a very important the secondary and tertiary c¢ precipitates, were carried
consideration, which must be carefully examined and out. After the heat treatment, specimens were exposed at
assured before putting them to use. temperatures of 800 C, 850 C, and 900 C for times of
Superalloys generally experience various microstruc- 1000, 3000, 5000, and up to 10,000 hours, respectively.
tural changes during their service life, including c¢ For each exposure condition at least four specimens
coarsening, formation of a continuous GB carbide were prepared for tensile- or stress-rupture tests (two for
network, topologically close-packed (TCP) phase for- tensile-rupture tests and two for stress-rupture tests).
mation, and MC carbide degeneration.[2–6] These pro- Tensile- and stress-rupture tests (gage length 50 mm,
cesses remove much of strengthening elements from the gage diameter 5 mm) were performed at 900 C and
c matrix and significantly degrade the properties of the 900 C/201 MPa, respectively. Each rupture value,
alloys, such as mechanical properties, corrosion resis- including strength and elongation, represents an average
of at least two test results.
The microstructures were examined using optical
X.Z. QIN, Student, J.T. GUO, Professor, and C. YUAN, Associate
Professor, Superalloys Division, Institute of Metal Research, Chinese
microscope (OM) and scanning electron microscope
Academy of Sciences, Shenyang 110016, P.R. China and C.L. CHEN, (SEM). Chemical etching was employed for the general
Student, and H.Q. YE, Academician, are with Shenyang National microstructural observation using a solution containing
Laboratory for Materials Science, Institute of Metal Research, Chinese 20 g CuSO4, 50 mL HCl, and 100 mL H2O, which
Academy of Sciences, Shenyang 110016, P.R. China. Contact e-mail: dissolves c¢. Deep etching with an electrolyte of 200 g
[email protected]
Manuscript submitted December 18, 2006. KCl + 50 g citric acid + 200 mL HCl + 1000 mL
Article published online November 7, 2007 H2O, which removes the c matrix, was conducted for

3014—VOLUME 38A, DECEMBER 2007 METALLURGICAL AND MATERIALS TRANSACTIONS A

the three-dimensional observation of c¢. The specimens thermal exposure, these constitutional phases undergo
worked as the anode while the cathode was a stainless significant microstructural changes, resulting in severe
steel plate; the current density was ~0.5 A/cm2. Trans- modification of mechanical properties.
mission electron microscopy (TEM) equipped with an
energy dispersive X-ray spectroscope (EDS) was used
for phase identification. Foils for TEM were prepared A. Microstructural Evolutions
on a twin-jet electropolisher with a solution of 10 pct 1. c¢ Coarsening
perchloric acid and 90 pct ethanol at -25 C. As demonstrated in Table I, the lattice parameter (ac)
The room-temperature lattice parameters of the c¢ and of the c matrix declines during long-term thermal
c phases were determined by X-ray diffraction methods. exposure though scatter exists. Especially a significant
The c¢ phase was extracted using the electrolyte of 10 g reduction occurs within the exposure time of
(NH4)2SO4 + 15 g tartaric acid + 1200 mL H2O. 1000 hours. In contrast, the parameter (ac¢) of the c¢
Slices (12 mm in diameter, 4 mm in thickness) of heat- precipitates basically remains unchanged in the whole
treated and thermally exposed specimens were chemi- period of exposure. As a result, the magnitude of the c-c¢
cally etched for about half a hour in order to remove the misfit, according to Eq. [1], first presents a sharp drop
c¢ phase on the surface of the slices; then, the lattice within 1000 hours exposure and then a mild decrease
parameter of the c phase was approximately estimated when exposure time is longer than 1000 hours. The
by diffracting the etched slices. The (311)c and (331)c¢ precipitation of secondary phases (e.g., M23C6-c¢ cell
reflection peaks were used for the calculation of lattice and g, as depicted later) from the c matrix may be
parameters of the c and c¢ phases, respectively. Silicon responsible for the reduction of ac. That is, as the
was used as a standard for calibration. Lattice misfit d is secondary phases precipitate, alloying elements escape
defined by from the c lattice and result in its shrinkage.
d ¼ 2 (ac0
ac )=(ac0 þ ac ) ½1 In Ni-base superalloys, the morphology of c¢ particles
depends both upon the magnitude of the c-c¢ misfit and
where ac¢ and ac are the unconstrained lattice parameters the size of the particles.[7–10] Under the heat-treatment
of the c¢ and c phases, respectively. condition, the investigated alloy has a large c-c¢ misfit
The size and volume fraction of precipitates were (-0.35 pct), which makes the secondary c¢ precipitates
measured using image analysis software. Each measured having a considerable average size (305 nm) tend to be
value was an average of 50 readings obtained from 50 cuboidal in shape for minimizing the elastic energy
different images. (Figure 1). However, during long-term thermal expo-
sure, the secondary c¢ precipitates always assume a
spherical appearance, because of the extremely small
III. RESULTS AND DISCUSSION misfits (Table I), in order to minimize the c/c¢ interfacial
energy (Figure 2).
The microstructure of heat-treated K452 alloy con- For Ni-base alloys, precipitate alignment is under-
sists of c matrix, c¢ precipitate, c-c¢ eutectic, primary MC stood in terms of the minimization of the elastic
carbide, and GB M23C6 carbide. During long-term interaction energy, which is a function of not only the

Table I. Lattice Parameters of the c and c¢ Phases and the c-c¢ Misfits under the Conditions of Heat Treatment and 900 °C
Thermal Exposure

Heat Treatment 900 C/1000 h 900 C/5000 h 900 C/10,000 h

ac¢ (Å) 3.5904 3.5902 3.5901 3.5901
ac (Å) 3.6029 3.5891 3.5923 3.5876
d (pct) -0.35 0.03 -0.06 0.07

Fig. 1—SEM images of c¢ precipitates in the heat-treated specimen: (a) chemically etched and (b) electrolytically etched. The secondary and
tertiary c¢ precipitates are clearly visible in the insert.

METALLURGICAL AND MATERIALS TRANSACTIONS A VOLUME 38A, DECEMBER 2007—3015

Fig. 2—Secondary c¢ precipitates in the specimens exposed at 900 C for (a) 1000 h, (b) 5000 h, and (c) 10,000 h. Deep etching technique is used
for the three-dimensional observation of the c¢ precipitates.

lattice misfit between the precipitates and the matrix interface, suggesting that a classical decomposition
but also the size and volume fraction of the precipi- reaction, that is MC + c fi M23C6 + c¢, is operative
tates.[10–12] In this alloy, the alignment does not occur there (Figure 4(a)). As the reaction proceeds, the MC
under the heat-treatment condition, because of the acts as the source of C and Ti, while the c matrix serves
relatively minor volume fraction (13 pct) of the second- as the source of Ni, Al, and Cr.
ary c¢ precipitates (Figure 3(b)). Similarly, neither the With the accumulation of c¢ and M23C6, the exchange
alignment is present during long-term thermal exposure, of alloying elements between the primary MC and the c
due to the sharp drop of magnitude of the c-c¢ misfit matrix becomes increasingly difficult. Nevertheless,
(Table I). In these two cases, the elastic interaction because Ni diffuses through the obstacle of the c¢-
energy is low, which may be the essential reason why the M23C6 film more easily than Al and Ti,[16,17] it combines
secondary c¢ precipitates do not align in the present with Ti to form the g (or Ni3Ti) phase at the interface
alloy, unlike many other superalloys.[8,13,14] between the film and the MC (Figure 4(b)). The g phase
The size and volume fraction changes of the second- depletes the c¢ forming elements (principally Ni and Ti),
ary c¢ precipitates at the exposure temperatures of consequently suppressing c¢. Therefore, the form of
800 C, 850 C, and 900 C are shown as functions of primary MC degeneration can now be written as MC +
exposure time in Figures 3(a) and (b), respectively. It is c fi M23C6 + g at the intermediate stage of thermal
clear that the coarsening rate of the secondary c¢ exposure, which was once reported in Reference 6.
precipitates increases with exposure temperature, and Finally, during the late stage of exposure, the diffusion
that their volume fraction goes up with exposure of alloying elements, especially the high atomic number
temperature or time. Also, one can understand that W and Mo atoms, is further blocked by the ordered g
both the dissolution of tertiary c¢ precipitates and the phase. As a result, W and Mo are enriched locally within
redistribution of alloying elements under nonequilibri- the reaction region, facilitating the formation of the
um conditions are in fact responsible for the increase in a-(W, Mo) phase that is sporadically embedded in
the size and volume percentage of the secondary c¢ the slight-gray g phase (Figure 4(c)). The presence of
precipitates. the a-(W, Mo) phase establishes the operation of another
MC decomposition reaction that can be summarized into
2. Primary MC Degeneration MC + c fi M23C6 + a-(W, Mo) + g.
In heat-treated specimens, most primary MC carbides It should be pointed out that M23C6 is always one of
(M represents Ti, W, and Nb; Table II) with an average the transformation products in the whole process of
size of 6.92 lm have an irregular blocky morphology primary MC degeneration, for C diffuses much faster
and are located both at the GBs and in the interdendritic than any other element and can relatively easily combine
regions. During long-term thermal exposure, these with Cr at any stage of thermal exposure mentioned
carbides deteriorates severely and various transforma- previously. The EDS measurements of various phases
tion products are sequentially present on their periph- involved in the process of primary MC degeneration are
eries with exposure, as illustrated in Figure 4.[15] shown in Table II.
Initially, a thin layer of c¢ decorated with small and The various phase interfaces, such as M23C6/c¢, g/MC,
discrete Cr-rich M23C6 particles emerges at the MC/c and g/c¢, are formed in the process of primary MC

3016—VOLUME 38A, DECEMBER 2007 METALLURGICAL AND MATERIALS TRANSACTIONS A

 of degenerated, coarse, and irregular MC carbides
distributed at the GBs are especially more detrimental
than when they are in the GIs.

3. Precipitation and Evolution of M23C6 Carbides

within GIs
M23C6 carbides dendritically precipitate from the
supersaturated c matrix and coarsen during thermal
exposure. Their average size is both temperature and
time dependent: For a given exposure temperature, the
size increases and gradually approaches a critical value
with time; and, the higher the exposure temperature, the
larger the critical size.[21]
The precipitation of M23C6 carbides rich in Cr, W,
and Mo leads to the local enrichment of c¢ forming
elements, such as Ni, Al, and Ti and then the presence of
the c¢ precipitates, forming an M23C6-c¢ eutectoid cell.[21]
In the cell, initially the M23C6 carbide is dendrite-shaped
and the c¢ precipitates are embedded in the carbide
dendrite. Under different thermal exposure conditions,
the M23C6 carbide undergoes various degrees of mor-
phological changes: At 800 C, it basically exhibits a
dendritical appearance through the entire period of
exposure; while at 850 C, its morphology tends to
transform from flowerlike dendrite to irregular block.
However, the most notable morphological transition
occurs at 900 C, as illustrated in Figure 5, where the
M23C6 carbide evolves in shape from flowerlike dendrite
to irregular block to regular polyhedron; meanwhile, the
c¢ precipitates embedded in the M23C6 dendrites migrate
outward and agglomerate gradually into a spherical c¢
envelope encircling the central carbide.
It should be pointed out that the minimization of the
M23C6/c¢ interphase boundary energy is actually the
driving force of the morphological evolution of M23C6
carbides, as described in Reference 21.
Regardless of size and shape, M23C6 can act as a
strong barrier to mobile dislocations and stacking faults
Fig. 3—Increases in the (a) diameter and (b) volume fraction of the that have cut through the c¢ envelope around the
secondary c¢ precipitates with exposure time at various exposure carbide.[21] However, the following aspects determine
temperatures.
the inappreciable influence of M23C6 on mechanical
properties: (1) the population of M23C6 is small, less
deterioration. Under the applied load, these interfaces, than 1.3 pct in volume fraction; (2) the precipitation and
because of high stress concentration and interfacial coarsening of M23C6-c¢ cells remove much of solid
energy, tend to become the favored initiation sites and solution strengthening elements, that is, Cr, W, Mo, Al,
propagation paths of microcracks.[15] Because micro- and Ti, from the c matrix and weaken the alloy;[5,22] and
cracks promote the fracture of superalloys and contrib- (3) M23C6 particles mainly distribute in the interden-
ute to the reduction of service life,[5,18–20] MC dritic regions and often crowd in the form of loops,
degeneration, which results in more frequent cracking chains, or clusters, as demonstrated in Figure 6, so that
than the intact MC, is undoubtedly deleterious to the their resistance to dislocation motion is discounted
thermally exposed K452 alloy. A considerable amount severely.

Table II. EDS Results of Various Phases Involved during the Primary MC Degeneration (Weight Percent)

Co Cr Al Ti W Nb Mo Ni
c 14.00 26.60 1.41 2.23 3.64 — — 52.12
MC 0.64 1.27 — 46.75 26.37 16.55 1.85 6.57
c¢ 4.22 4.64 10.47 10.42 1.22 — — 69.03
M23C6 2.23 65.08 0.75 1.97 10.70 — 2.23 17.04
g-(Ni3Ti) 5.83 2.44 1.53 13.35 4.20 3.74 — 68.91
a-(W, Mo) 1.76 1.72 0.24 3.21 72.97 1.01 4.25 14.84

METALLURGICAL AND MATERIALS TRANSACTIONS A VOLUME 38A, DECEMBER 2007—3017

Fig. 4—Backscattered electron images of degenerated MC carbides under the different exposure conditions: (a) through (c) thermal exposure of
800 C/1000 h, 850 C/5000 h, and 900 C/10000 h, respectively.[15]

Fig. 5—Morphologies of M23C6 carbides in the specimens exposed at 900 C for (a) 1000 h, (b) 5000 h, and (c) 10,000 h.

4. Evolution of GB Microstructure chain and thickens with the rise of exposure temperature
The GB phases observed in this investigation are c¢ or time.
precipitate, M23C6 carbide, and infrequently primary It is well accepted that blocky, closely spaced M23C6
MC carbide. In the heat-treated specimen, the GBs are particles engulfed in c¢ improve rupture life and
fine, as there is only a small quantity of M23C6 particles ductility by hindering GB sliding, thereby reducing
and c¢ precipitates present (Figure 7(a)). However, nucleation and growth of cavities;[4,23–25] however, the
during long-term thermal exposure the GBs coarsen presence of a wide and continuous M23C6 chain
through the following possible processes (Figure 7(b) sandwiched by two layers of c¢ may facilitate crack
through 7(e)): (1) the small discrete M23C6 particles at propagation and lead to tensile and notch brittle-
the GBs grow and gradually interlink into a thin ness.[4,24] Hence, an optimum GB M23C6/c¢ structure
discontinuous, and then a coarse continuous chain; where blocky M23C6 particles are engulfed in c¢ as
and (2) a continuous c¢ film forms on either side of the densely as possible is desirable.[26–29]

3018—VOLUME 38A, DECEMBER 2007 METALLURGICAL AND MATERIALS TRANSACTIONS A

Fig. 6—Inhomogeneous distributions of M23C6 carbides in the 900 C/10,000 h thermal exposure specimen: (a) loops, (b) chains, and (c) clusters
of M23C6 carbides.

Fig. 7—GBs under the (a) heat treatment and (b) thermal exposure conditions of 800 C/1000 h, (c) 850 C/5000 h, (d) 900 C/5000 h, and (e)
900 C/10,000 h.

METALLURGICAL AND MATERIALS TRANSACTIONS A VOLUME 38A, DECEMBER 2007—3019

 The c¢-free zones do not occur along the GBs in the
present alloy. The reason is probably that the alloy is
subjected to a correct heat-treatment regimen, that is, a
solution anneal (4 hours at 1170 C) followed by a high-
temperature aging (4 hours at 1050 C) and then a low-
temperature aging (16 hours at 850 C). The triple heat
treatment makes Cr distribute uniformly across the
GBs, suppressing the Cr-depletion zones, and accord-
ingly suppresses the c¢-free zones.[30–32] Generally, the c¢-
free zones are present only when the alloys are subjected
to a dual heat treatment (a solution anneal followed by
lower temperature aging), which results in a Cr deple-
tion zone with a steep Cr concentration gradient along
the GBs. The Cr lowers the solubility of c¢ forming
elements, so its depletion adjacent to the GBs leads to
the dissolution of the c¢ precipitates forming the c¢-free
zones,[33–35] which are generally thought to be deleteri-
ous to the properties of the alloys.[36,37]

5. g Phase
At the exposure temperatures of 800 C and 850 C, a
small quantity of needle-shaped g phase precipitates
from the c matrix, whereas at 900 C, there is almost no
g phase present.
Cracks that initiated from the g phase and extended
into the matrix were not observed. Considering the small
population of the g phase, its influence on mechanical
properties is negligible.

B. Degradation of Mechanical Properties

The properties of c¢-strengthened alloys depend on
many factors, such as volume fraction and size of c¢,
solid-solution strengthening of c, and presence of hyper-
fine c¢.[26] However, these factors are modified during
thermal exposure in the present experiment, for example, Fig. 8—Tensile-rupture properties of thermal exposure specimens:
leading to the coarsening of the secondary c¢ and the (a) tensile strengths and (b) tensile elongation.
absence of the tertiary c¢, which cause a significant loss of
tensile strength of the alloy (Figure 8(a)). It should be
emphasized that although the volume fraction of the
secondary c¢ increases with exposure (Figure 3(b)), it tends to cause the premature onset of intergranular
does not provide an essential improvement to the fracture and therefore reduces the elongation. This
strength, for it not only results in virtually no new c¢ is especially true when a considerable amount of
nucleus, but also withdraws solid-solution strengthening degenerated MC carbides that facilitate the initiation
elements from the c matrix. of microcracks distribute themselves at the GBs
Almost all the tensile or stress-rupture specimens (Figures 8(b) and 9(b)).
failed exclusively along the GBs perpendicular to the
applied load in the present study. Therefore, the GBs
with a M23C6/c¢ structure are crucial to the rupture
IV. CONCLUSIONS
properties, namely rupture life and strain. During
thermal exposure the stress-rupture lives of specimens 1. The secondary c¢ precipitates are cuboidal in shape
rise first with the density of the GB M23C6 particles and in the heat-treated specimens, whereas they assume
then decrease due to the development of a continuous a spherical appearance during long-term thermal
carbide chain as well as c¢ coarsening, as presented in exposure. As they coarsen, the secondary c¢ precipi-
Figure 9(a). A life peak always occurs at a certain tates increase in volume fraction. The c¢ coarsening
exposure time, which may correspond to an optimal is the principal reason for the reduction of strength
M23C6/c¢ structure at the GBs; the higher the exposure of the alloy.
temperature, the earlier the occurrence of the peak. 2. The evolution of GB microstructure has a signifi-
The c¢ coarsening widens the c channels and facilitates cant effect on the stress-rupture life, which first rises
the movement of mobile dislocations. Therefore, it is with the density of GB M23C6 particles and then
beneficial to the elongation of the alloys. However, the decreases due to the formation and growth of con-
formation of a continuous M23C6 chain at the GBs tinuous carbide chains. A peak occurs when the

3020—VOLUME 38A, DECEMBER 2007 METALLURGICAL AND MATERIALS TRANSACTIONS A

 ACKNOWLEDGMENTS
The authors thank Professor X.X. Jiang and
Dr. J.S. Hou, Institute of Metal Research, Chinese
Academy of Sciences, for their helpful discussions.

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