312 Chiang Mai J. Sci.

2009; 36(3)

Chiang Mai J. Sci. 2009; 36(3) : 312-319

www.science.cmu.ac.th/journal-science/josci.html
Contributed Paper

Gamma Prime Phase Stability after Long-Term

Thermal Exposure in Cast Nickel Based Superalloy,
IN-738
Panyawat Wangyao* [a], Nutthida Chuankrerkkul** [b], Sureerat Polsilapa [c],
Ponlit Sopon [c] and Weerasak Homkrajai [d]
[a] Department of Metallurgical Engineering, Faculty of Engineering, Chulalongkorn University,
Bangkok 10330, Thailand.
[b] Metallurgy and Materials Science Research Institute, Chulalongkorn University, Bangkok 10330, Thailand.
[c] Department of Materials Engineering, Faculty of Engineering, Kasetsart University,
Bangkok 10900, Thailand.
[d] Electricity Generating Authority of Thailand, Nonthaburi 11130, Thailand.
*Author for correspondence; e-mail: panyawat@hotmail.com; e-mail: nutthita.c@chula.ac.th

Received: 13 January 2009

Accepted: 20 March 2009
ABSTRACT
Long-term isothermal exposure tests were conducted on IN-738 alloy to evaluate
the variation of gamma prime particle coarsening behavior after different rejuvenated heat
treatment conditions. The long-term exposure tests (up to 2,500 hours) were conducted at
two temperatures (900oC and 1,000oC) to assess gamma prime particle coarsening behavior.
Metallographic work was performed on isothermally aged samples to characterize gamma
prime coarsening as a function of aging time and temperature. At all aging temperatures and/
or times investigated, the gamma prime particles in all tested specimens were more coarsening
than the initial reheat treated ones. The gamma prime particles appeared to be more coarsening
into round shape or agglomerated between them comparing to the initial ones of each reheat
treatment. The degree of coarsening, as evidenced by gamma prime particle size, increased
with increasing heating time and temperature. In most cases, the amount of secondary or very
fine gamma prime precipitates decreased with increasing heating temperature and finally
disappeared. It was found that the lower solutioning temperature provided the higher rate of
γ coarsening at both elevated temperatures. In contrast, the higher solutioning temperature
kept slow rate of γ coarsening resulting in lower average γ particle size.
Keywords: rejuvenation, re-heat treatment, microstructural repair, gamma prime particle
coarsening, and nickel-based superalloy.

1. INTRODUCTION
Nickel based superalloys are structural
materials with chemical composition and
structure, which have been developed to
enable the use at high temperature applications.
The microstructures and mechanical properties
(for both low and high temperatures) can be
related to their manufacturing processes. One
of these processes is heat treatment, which
solution treatment in most cases, followed
by a single or a double aging sequence to
Chiang Mai J. Sci. 2009; 36(3)
precipitate homogeneous distributions of
either cuboidal or spherical gamma prime
within the grains interior as well as discrete
grain boundary carbides [1]. Full solution
treatment or partial solution treatment
temperatures including aging treatments have
been developed and modified to optimize the
completed precipitation of gamma prime
phase in matrix.
The size, volume fraction and distribution
of gamma prime phase are vital to control the
creep strength at high to intermediate stresses.
The proper reheat-treated microstructure can
provide their phase stability, and adequately
high strength and good ductility even after
long-term thermal exposure. The mechanical
property behaviors of superalloys are very
strongly related to the alloy microstructures
[2-6]. The superalloy microstructures
continually change with time at the elevated
temperatures. In the new, heat treated alloy,
the gamma prime (γ ) particles are arranged
in a structure, which results in an optimum
balance of tensile, fatigue, and creep properties
[7-10].
It is generally known that mechanical
properties are related to the microstructures.
Therefore, many previous research works
[3-11] had been carried out to investigate the
relationships of microstructure and mechanical
properties. However, the use of these expensive
materials requires a repair process providing
the re-establishment of the initial properties
and the original microstructure of the long-
term used or damaged parts for the economic
reason. The heat-treatment processes for
nickel-based superalloys continue to change
in order to optimize numerous mechanical and
physical properties [5-9]. This allows making
the selection of heat treatment parameters
increasingly challenging.
The cast nickel-based superalloy IN-738
is used as a blade material in the first row
high-pressure stage of gas turbines. The alloy
313
contains refractory elements such as Mo, W,
Ta, Cr and Co to prevent local hot corrosion
[10]. The alloy has a multi-phase microstructure
consisting FCC γ matrix, bimodal γ’ precipitates
(primary and secondary), γ-γ eutectic, carbides
and a small amount of deleterious phases such
as σ, δ, η and Laves. The total weight percent
of γ’ in IN-738 superalloy is higher than 60%
[11]. Therefore, the high-temperature strength
of the alloy depends strongly on γ properties.
According to the previous work [12], the
rejuvenation process provides blades to
double and, in some cases, triple the lifetime
as compared to the original ones. For alloys
such as IN-738, IN-792, U-500, X-750 and
the newer alloys such as GTD 111, GTD-
111DS, R80DS, and IN-939, which are used
in many land-based gas turbines, have been
rejuvenated and successfully returned to
service according to the previous information
of LIBURDI Engineering Company Limited,
Canada. In each case, the blades were creep
life expiry when received for processing and
then giving reliable service after rejuvenation.
The aim of this research work is to
determine the most suitable and practicable
repair-condition, which could restore micro-
structure and provide the most microstructural
stability after long-term thermal exposure for
gas turbine blades made of casting nickel based
superalloy grade IN-738 after 50,000-hour
service operated by Electricity Generating
Authority of Thailand (EGAT).
2. MATERIALS AND METHODS
The cast nickel base superalloy in this study
was IN-738 (see chemical composition in
Table 1). Rectangular plates, having a
dimension about 1 cm2 were cut from the most
severe degradation zone of turbine blades.
Specimens were heat treated according to heat
treatment conditions including solution treatment,
primary and secondary precipitation aging
treatments in vacuum furnace. The details of
314 Chiang Mai J. Sci. 2009; 36(3)

experimental heat treatments are shown in hours in order to investigate the coarsening
Table 2. Then reheat treated specimens after behavior of gamma prime particles after
each condition were heated at both 900 oC and various reheat treatments.
1,000 oC for 500, 1000, 1500, 2000, and 2500 All sectioned samples after each aging

Table 1. Chemical composition in weight % of IN-738.

Ni Cr Co Ti Al W Mo Ta Nb C Fe B Zr
Bal. 15.84 8.5 3.47 3.46 2.48 1.88 1.69 0.92 0.11 0.07 0.12 0.04

Table 2. Heat treatment conditions applied to long term exposed IN-738.

Condition Solution Primary Secondary
No. Treatment precipitate aging precipitate aging
1* 1125oC/ 2hr. (AC) - 845oC/ 24 hr. (AC)
2 1125oC/ 2hr. (AC) 925oC/ 1 hr. (AC) 845oC/ 24 hr. (AC)
3 1125oC/ 2hr. (AC) 1055oC/ 1 hr. (AC) 845oC/ 24 hr. (AC)
4 1175oC/ 2hr. (AC) - 845oC/ 24 hr. (AC)
5 1175oC/ 2hr. (AC) 925oC/ 1 hr. (AC) 845oC/ 24 hr. (AC)
6 1175oC/ 2hr. (AC) 1055oC/ 1 hr. (AC) 845oC/ 24 hr. (AC)
* Standard Heat-Treatment condition.

were ground and polished using standard
metallographic techniques and were sub-
sequently etched in marble etchant. The
etchant’s chemical compositions are: 10 g.
CuSO4, 50 ml HCl, and 50 ml H2O. The
microstructures of heat treatment samples
were study by scanning electron microscope
with secondary electron mode and Image
Analyzer. The size and volume fraction of
gamma prime particles were determined.
3. RESULTS AND DISCUSSION
3.1 As-received Microstructure
The SEM photograph, obtained from the
transverse sections at about mid blade
height of the airfoil, is shown in Figure 1a.
The microstructure of as-cast alloy generally
consists of extensive precipitation of ordered
L12 γ intermetallic phase within dendrite
core and in the interdendritic region. The
agglomerated gamma prime particles can
be seen. Coalescence of the primary and
secondary gamma prime particles, as result of
long-term service, seems to occur resulting in
larger and rounded particles. However, carbide
and/or gamma prime phases normally lowers
ductility or toughness of blade alloy. This can
lead to lower creep strength and impact
resistant of the blades.
In this study, the airfoil microstructure
showing significant degradation in service,
the coarse gamma prime particle size was
about 1.2 micron. The primary gamma prime
particles have spheroidized and secondary
gamma prime coarsened in the airfoil samples.
This type of microstructure is theoretically
expected to have low efficiency to block
dislocation movements during loading at high
temperatures resulting in lower creep
resistance. Therefore, it is needed to recover
Chiang Mai J. Sci. 2009; 36(3)
microstructure to the same as or similar to
the original one by simple reheat treatment
processes.
3.2 The Microstructures of Reheat-treated
Alloy
According to the previous works [7-8,
13], repeating the standard heat treatment
sequence does not always work well. The
structure and properties were not fully
recovered by this refurbishment treatment
applied to these IN-738 blades. It is reported
that the microstructure was only partially
recovered by such simple reheat treatment.
However, when reheat treatment condition,
according to No.1 (standard heat treatment),
was applied to long-term exposed specimen
in this study, the more homogeneous
microstructure consisting of uniform dispersion
of finer gamma prime precipitates was
obtained. The size of γ precipitate particles
are uniform and similar in size and shape,
Figure 1b. This type of microstructure is
previously expected and theoretically desired
as the most optimized microstructure, which
could provide very good mechanical properties
at elevated temperatures, especially, for both
short-term strength at elevated temperature
and high creep resistance.
According to heat treatment of program
No.2, It was found that the morphology is
different from the standard heat-treated one.
Primary precipitate aging at 925oC for 1 hour
resulted in an early precipitation of gamma
prime γ particles. After secondary precipitate
aging, elements needed to form γ precipitate
would more diffuse into the former gamma
prime precipitates causing the coarsening of
these precipitates during secondary aging
resulted in coarser size. Such kind of
microstructure could probably provide good
rupture and/or creep resistance in some
degree. As it is already well known that creep
strength of alloys by γ precipitation is a
315
function of γ particle size. It can be concluded
that temperature of 925oC as primary aging
produced more uniform and coarser of
rounded-γ particles.
The microstructure after heat treatment
according to program No.3 shows the
bimodal microstructure of non-uniform
dispersion of both coarse and very fine
gamma prime precipitates. The coarse gamma
precipitates are in round shape at the proper
size. Effect of primary precipitate aging at
1,055oC for 1 hour resulted in more coarsening
of both sizes of gamma prime particles with
higher volume fraction of γ -phase after secon-
dary aging comparing to the reheat-treated
microstructure of programs No. 1 and 2, which
has lower amount of precipitated coarsening
particles. Specimens from programs No. 4-6
received the effect of the highest solutioning
temperature on final microstructures. This
highest solutioning temperature provided the
microstructure with much lower driving force
for coarse γ phase precipitation during aging
resulting in very low volume fraction of
coarse γ precipitated particles. The inserted
primary aging could not strongly influence to
the size, distribution and volume fraction of
coarse γ particles but do greatly to the very
fine one.
3.3 Microstructures after Long-term
Exposures
Heating at both temperatures resulted in
drastically coarser gamma prime particles as
compared to the initially received reheat-treated
specimens as shown in Figures 1c and 1d, and
presented by conditions 1-6 in Figures 2-5,
which are referring to condition No. 1-6 in
Table 2, respectively. However, in Figures 1c,
1d, 2 and 4, it could be clearly seen that the
higher heating temperature of 1,000 o C
provided the much higher coarsening rate of
gamma prime particles than of the lower one
(900oC) due to the difference in kinetics. The
316 Chiang Mai J. Sci. 2009; 36(3)

gamma prime particles greatly more coarsened
into round shape than those in each initially
reheat treated specimens. In the alloy, the
degree of coarsening, as determined by
gamma prime particle size, increased with
both increasing heating temperature and time.
At each heating temperature, the size of
gamma prime particles increased, and the area
fraction of gamma prime particle decreased with
increasing heating time. It was also observed
that an increasing heating temperature
resulted in lower amount of gamma prime
precipitation.
During long-term heating, secondary
gamma prime particles would dissolve into
the matrix and then diffused to agglomerate
with the coarse gamma prime particles.
Considering the coarsening behavior of
gamma prime particles at 900oC and 1,000oC
(Figures 2 and 4), it was found that the
microstructures under previous reheat treatment
of conditions No. 5 was the most stable ones
due to the slowest coarsening rate of gamma
prime particles. When considering Figures 3
and 5, it could be seen that the area fraction of
total gamma prime particles of specimen

(a) (b)

(c) (d)
Figure 1. SEM micrographs of a) As-received microstructure after long-term service, b)
After standard heat-treatment at 1,125oC / 2hr. (AC) and 845oC / 24 hr. (AC); Condition
No. 1, c) After long-term exposure at 900oC for 2,500 hours; Condition No. 1 and d) After
long-term exposure at 1,000oC for 2,500 hours; Condition No. 1.
Chiang Mai J. Sci. 2009; 36(3) 317

under all reheat treatment conditions reduction of area fractions of gamma prime
continuously decreased with heating time. It particles comparing to those of the lower
was also found that the higher heating temperature.
temperature of 1,000oC resulted in faster

0 500 1,000 1,500 2,000 2,500 3,000

Heating time (hr)

Figure 2. The relationship between heating time and average size of gamma
prime particles at 900oC.

0 500 1,000 1,500 2,000 2,500 3,000

Heating time (hr)

Figure 3. The relationship between heating time and average area fraction of
precipitated phase at 900oC.
318 Chiang Mai J. Sci. 2009; 36(3)

0 500 1,000 1,500 2,000 2,500 3,000

Heating time (hr)

Figure 4. The relationship between heating time and average size of gamma
prime particles at 1,000oC.

0 500 1,000 1,500 2,000 2,500 3,000

Heating time (hr)

Figure 5. The relationship between heating time and average area fraction
of precipitated phase at 1,000oC.

4.CONCLUSIONS
1. The reheat-treated microstructure
according to program No. 5 provided the
most precipitated phase stability in term of
minimum coarsening rate after long-term
exposure at both 900oC and 1,000oC.
2. In almost reheat-treated microstruc-
tures, average area fractions of gamma prime
phase clearly decreased with heating time.
Chiang Mai J. Sci. 2009; 36(3) 319

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