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The Mechanism of η Phase Precipitation in A286 Superalloy During Heat

Treatment

Article  in  Journal of Materials Engineering and Performance · May 2013

DOI: 10.1007/s11665-013-0592-1

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The Mechanism of g Phase Precipitation in A286

Superalloy During Heat Treatment
M. Seifollahi, S.H. Razavi, Sh. Kheirandish, and S.M. Abbasi

(Submitted February 7, 2012; in revised form March 22, 2013)

In this research, the mechanism of eta (g-Ni3Ti) phase precipitation in iron-nickel-based A286 superalloy
was assessed during aging heat treatment in the temperature range between 650 and 900 °C for the times of
1-30 h. Optical microscopy, scanning electron microscopy, differential thermal analysis, and x-ray dif-
fractometry were used to describe the g phase transformation. The results showed that the major pre-
cipitates at temperatures below 840 °C were c¢ and g. The g phase started to precipitate at the expense of
the c¢ phase after prolonged aging. The g phase existed in the samples aged at temperature higher than
760 °C with cellular morphology. The g volume fraction increased with increasing heat treatment time. In
addition, when the aging temperature was increased from 760 to 820 °C, the g volume fraction increased
and then decreased after 840 °C. The g phase morphology also changed from cellular to Widmanstätten-
type during aging. The time-temperature-precipitation diagrams of these morphologies are presented. The
results indicated the differences in precipitation mechanisms of g phase at 840 and 860 °C.

grain boundary migration under this situation. On the other

Keywords A286 superalloy, heat treatment, TTP diagram, g
phase
1. Introduction
A286 is an austenitic iron-nickel-based superalloy that is
widely used in the gas turbine industry at intermediate elevated
temperature service. This alloy is strengthened by the spherical-
ordered face-centered cubic (fcc) c¢ Ni3(Al,Ti) precipitates
(Ref 1, 2). The c¢ phase is unstable after aging treatment at high
temperature and dissolves to precipitate the stable g (hcp
Ni3Ti) phase (Ref 3). The investigation on Ni-based superalloys
such as Nimonic 263 revealed c¢-free zones surrounding each g
precipitate, which indicated that the g phase was formed at the
expense of the c¢ phase (Ref 4). There is a phase transformation
of c¢ fi g in the A286 after a long aging time (Ref 5-7).
The precipitation behavior of the g and c¢ phases in A286
superalloy is important for achieving excellent mechanical
properties (Ref 8). Hot rolling above the solvus temperature of
these two precipitates probably leads to precipitation of g phase
as well as fine and dispersed c¢ phase during the air cooling
process. The formation of the fine blocky g at the grain
boundaries may also enhance high temperature properties of the
alloy. This may also be explained considering the difficulty of
M. Seifollahi and S.H. Razavi, School of Metallurgy and Materials
Engineering, Iran University of Science and Technology (IUST),
Narmak, 16846-13114 Tehran, Iran; Sh. Kheirandish, School of
Metallurgy and Materials Engineering, Iran University of Science and
Technology (IUST), Narmak, 16846-13114 Tehran, Iran; and Center
of Excellence for High Strength Materials, Iran University of Science
and Technology (IUST), Tehran, Iran; and S.M. Abbasi, Metallic
Materials Research Center (MMRC-MA), Tehran, Iran. Contact e-mail:
hrazavi@iust.ac.ir.
hand, the formation of Widmanstätten morphology deteriorates
the performance of the alloy for room temperature applications
requiring strength and ductility (Ref 9). The formation of
cellular g may also degrade the notch stress rupture strength of
Fe-based and Ni-based superalloys (Ref 10, 11). Therefore,
controlling the microstructure is a necessary requirement for
optimizing the properties of A286.
Although, many studies have been carried out on the
mechanism of precipitation (Ref 6, 12) and the effect of heat
treatment on g and c¢ phases (Ref 13, 14) in Fe-Ni-and Ni-Co-
based alloys, most of them discussed the kinetics of c¢ growth.
There is a lack of knowledge on the behavior of the g phase
during heat treatment. Thus, in the present work, the formation,
volume fraction, and morphology of the g phase formed during
heat treatment were investigated.
2. Experiments
The A286 superalloy used in this investigation was received
in the form of 80% hot-rolled slabs, 12 mm thick, with
chemical composition as follows: 25.8Ni-13.6Cr-1Mo-2.13Ti-
0.21Al-0.2V-0.1Si-Fe bal (wt.%). 10 9 10 9 10 mm3 speci-
mens were heat treated at temperatures in the range between
650 and 900 C for 1-30 h, in an electrical resistance furnace
with the accuracy of ±5 C for aging heat treatment studies.
Differential thermal analysis (DTA), on the model TGA/
SDTA85, was performed on 1 9 193 mm3 specimens. The samples
were heated in the temperature range between 450 and 1000 C,
with a heating rate of 20 C/min using Argon as the carrier gas.
Metallographic sections were prepared using standard
mechanical polishing procedures and etched with 15 mL HCl,
8 mL HNO3, and 4 mL glycerin solution. A Vega Tescan
scanning electron microscope (SEM) equipped with an energy
dispersive spectroscopy (EDS) analyzer operating at 15 kV and
an optical microscope (OM) were used to observe the

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Fig. 1 (a) SEM microstructure and (b) XRD pattern of the solu-
tion-annealed A286 superalloy
morphology and distribution of phases. The volume fraction of
g phase was calculated by Image Analyzer Clemex software.
The g phase was identified using the phase extraction
technique combined with x-ray diffraction (XRD). The phase
extraction was performed by the electrolytic method, immers-
ing the specimen in an electrolyte with a composition of 10%
HCl and 90% ethanol. The current density of electrolysis was
set at 0.1 A/cm2 for 16 h and a 316 stainless steel cathode was
used. The sediment was washed three times in ethanol and then
dried. A Phillips PW 1800 x-ray diffractometer (40 kV, 30 mA)
with CuKa radiation was used for XRD.
The hardness of the heat-treated samples was measured
using a Vickers hardness testing machine under 30-kg load.
Five indentations were made, and the average hardness was
used to plot the curves.
3. Results and Discussion
The SEM microstructure and XRD pattern of the solution-
annealed alloy are shown in Fig. 1(a) and (b), respectively. The
austenitic grains are visible in Fig. 1(a), and the XRD pattern in
Fig. 1(b) shows that there are only the peaks of c(Fe-Ni). No
Fig. 2 (a) SEM micrograph showing intragranular Ti(C,N) particles
after solution treatment and (b) EDS spectrum obtained from
Ti(C,N) shown in (a)
peaks of other phases can be seen due to dissolution of the
precipitates during solution annealing. The results indicate that
the matrix of the alloy is completely austenitic with equiaxed
grains and an average size of 42 lm. The grain size distribution
is peripherally inhomogeneous, indicating that some grain
growth has taken place. There are some annealing twins in
Fig. 1(a), which are a characteristic feature of low to medium
stacking fault energy (SFE) materials (Ref 15, 16). The SFE of
this alloy has been reported as 65-76 MJ/m2. The presence of
twins in both small and large grains indicates that twins are
generated during both the recrystallization and grain growth
steps in order to reduce the overall boundary energy of the
alloy.
Only a few inclusions are observed in the alloy after solution
treatment in Fig.1(a). As seen in Fig. 2(a), their maximum size
is about 4 lm, and they are mostly in the cubic and round
shapes. The EDS spectrum obtained from these particles, which
is shown in Fig. 2(b), indicates that these particles are Ti(C,N)
that dissolve some Fe, Ni, Cr, and Al. According to Ref 17,
these inclusions are primary titanium carbides and nitrides,
Ti(C,N), which are formed during solidification.
The solution-annealed alloy was analyzed by DTA to deter-
mine the phase formation or transformation during heating.
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Fig. 3 DTA heating curve of A286 superalloy; heating rate: 20 C/min
in Ar
Figure 3 shows the DTA results at a heating rate of 20 C/min
in the temperature range between 450 and 1000 C for A286
superalloy. There are two peaks and one valley in this curve.
The exothermic peak at 690 C, peak 1, can be for the
precipitation of c¢. The beginning of peak 1 at 615 C may
correspond to the start of the formation of c¢ phase. Beyond this
temperature, the alloy consists of a two-phase space, i.e.,
c + c¢. At this stage, the c¢ phase grows and its volume fraction
increases. Further increase in temperature leads to c¢ dissolution
which is followed by precipitation of g phase at valley 2
(825 C) by endothermic reaction. Rho and Nam (Ref 2)
demonstrated that the precipitation temperature of g phase is
about 840-870 C, and this transformation is endothermic. At
930 C, peak 3, the g phase dissolves. So, the alloy is
completely austenitic, as discussed in the previous section.
The microstructure of the alloy and the g phase precipitation
behavior during heat treatment were also studied. It can be seen
in Fig. 4(a) and (b) that in the samples which were heated at
840 C for 4 and 12 h, the g phase was formed in two different
morphologies, which will be described later. Figure 4(c)
represents the result of the EDS line scan across the white
phase and the matrix. High Ti and low Al peaks were found
corresponding to the white phase. Therefore, it can be
concluded that the white phase with cellular morphology is
the g phase. It is noticeable that the g phase shows a negligible
solubility for Al, which is in accordance with the result of Sims
et al. (Ref 18). The XRD of the extracted g phases in Fig. 4(d)
proves that the extracted phases are g phases. The electrolytic
solution dissolved the whole alloy, except the g phases.
The volume fraction of g phase, formed during aging, is
measured using Clemex software and the systematic manual
point count method (Ref 19), and the results are summarized in
Fig. 5. The microstructures of the alloys heat treated for 16 h in
Fig. 6(a) to (i) show the variation of g phase over the
temperature. According to these figures, the behavior of A286
superalloy during aging heat treatment is divided into four
temperature regions which are as follow; 1: under 760 C; 2:
between 760 and 840 C; 3: at 840 C; and 4: beyond 840 C.
The following is the investigation of the g phase in each region.
No detectable changes in the microstructure studied by SEM
or OM are observed by aging the solution-annealed samples at
temperatures less than 760 C, region 1. As illustrated in Fig. 5
and 6(a), there is no g phase in the alloy in this region which
correlates with DTA analysis. Further information about
microstructures can be discussed from the hardness tests.
Figure 7 summarizes the hardness results of all the samples
studied in Fig. 5. By aging at 650 C, a gradual but slow
Journal of Materials Engineering and Performance
increase in hardness with aging time can be observed. This may
correspond to the start of the precipitation of c¢ at 650 C.
Increasing the aging temperature to 720 C causes a significant
change in hardening response and the maximum value of 305
VHN can be achieved at 16 h. Formation of c¢ is responsible
for age hardening and increasing the hardness of the alloy. The
c¢ phases are shown in Fig. 6(b). Hence, the trend of age
hardening in Fig. 7 shows that c¢ forms at 650 C, but it does
not complete until 60 h (Hardness of the alloy aged at 650 C
for 60 h is 243 VHN which is not represented in Fig. 7) and the
age hardening is completed at 720 C for 16 h. This is in line
with the DTA results.
In region 2, at 760 C, the g phase starts to nucleate. This
temperature is lower than that observed in the DTA results,
which is due to the rate of increasing temperature that is higher
in the DTA system than in the aging treatment when the g
phase nucleates and grows. Therefore, the g phase precipitation
temperature in the DTA system is higher than in the aging
process. According to Fig. 5, at up to 4 h, no g phase forms at
760 C. After 8 h, a cellular g phase appears at the grain
boundaries. At region 2, the amount of g increases with time at
all temperatures. According to Fig. 6(c) to (f), the increase in
temperature causes a dramatic increase in the g volume
fraction. The amount of g formed by aging at this region, i.e.,
760, 780, 800, and 820 C for 16 h, is 0.3, 0.5, 2, and 2.8%,
respectively. Ti atoms diffuse to high energy areas and the g
phase will nucleate by increasing the time and temperature.
Furthermore, in the case of A286, the lattice misfit between the
c¢ phase and the matrix was reported as 0.45% when aged for a
shorter time and 0.5% for a longer time (Ref 3, 20). As a result,
by increasing the time, coarsening and coalescence of the c¢
phase occur. So, the coalesced c¢ dissolves and the phase
transition of c¢ fi g occurs. The evidences of this transfor-
mation can be seen in Fig. 8. As shown in this figure, there are
some areas between g lamellas where c¢ is absent. Moreover,
the c¢-free zone is extremely obvious in Fig. 4(b). These
indicate that the g forms at the expense of c¢. According to
Fig. 8, the c¢ size between g lamellas is about twice the size in
the matrix. It is evidence of c¢ coalescence, which is a result of
increasing aging time and temperature. Coalescence of c¢
particles releases the Ti as a result of diffusion increase.
Furthermore, aging causes an increase in the lattice misfit in the
c¢/c, so stacking fault can be generated into the c¢ (Ref 20, 21).
Forming stacking fault into the c¢ makes it unstable and causes
the c¢ fi g transformation. Heo et al. (Ref 7) investigated the
transformation of g phase to fcc austenite during isothermal
aging of the Fe-Ni-Ti alloy and suggested that the change of the
crystalline structure from g-D024 to c¢-L12 could occur by the
introduction of intrinsic stacking faults into the g phase.
In region 2, aging at 760 C and higher temperatures results
in an initial rise in hardness. After reaching a maximum value,
which shifts to shorter times with increasing temperature, the
hardness of the alloy starts to fall to lower values. The fall in
hardness after the peak may be attributed to the coarsening of c¢
precipitates and g phase formation (Ref 17). As c¢ becomes
more stable, the c¢ fi g transformation is retarded. The loss of
c¢ strengthening phase as a result of g formation is also
responsible for reducing the hardness. At temperatures higher
than 800 C and for prolonged aging, the hardness again starts
to increase. The reason for higher hardness is the formation of
Widmanstätten g.
According to Fig. 5, in region 3, and at the temperature of
840 C, the g percentages increase rather sharply to 0.5 and
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Fig. 4 (a) SEM microstructure of A286 superalloy aged at 840 C for 4 h (cellular g); (b) 840 C for 12 h (Widmanstätten g); (c) SEM EDS
line scan performed across an g phase and matrix; and (d) XRD of the extracted g phase

4
3.45% for 2 and 4 h, respectively. There is a maximum amount
Eta volume fraction (%)

of g at this temperature, and after that it falls to 2% at 8 h. 3.5

Consequently, there is a peak at 840 C for g formation on 4 h. 3
760
This phenomenon can be discussed from two points of view. 2.5
780
The first is the interaction between driving force of g formation 2 800
and Ti diffusivity. Precipitation and growth of g phase are
1.5 820
diffusion-type phase transformation processes, which largely
depend on enough titanium atoms and driving force for g 1 840

formation (Ref 8). It suggests that the diffusivity will increase 0.5 860
with temperature increase, but driving force will decrease and 0
result in the variation of the g volume fraction. The second may 0 5 10 15 20

be associated with the equilibrium state of g. It means that the
g phase is not the thermodynamic equilibrium phase and,
consequently, it transforms into c after prolonged aging. The
g fi c transformation was also reported by Heo et al. (Ref 7).
Therefore, the following transformation would happen during
aging: c fi c¢ fi g fi c.
It is not clear that above 800 C g forms from the c¢ fi g
transformation or this phase nucleates directly from austenite.
The authors are investigating this phenomenon by varying the
condition of aging heat treatment. The results of the two-step
aging heat treatment (First, the main c¢ precipitate is grown at a
temperature of 720 C for 16 h; subsequently, the second
treatment is performed at T > 720 C.) that is in progress
showed that the g volume fraction in this condition is far less
than in the one-step aging. This behavior illustrates that the
g phase is precipitated at the high temperature by two
Aging time (hour)
Fig. 5 Variation of the g volume fraction with time at different
aging temperatures in A286 superalloy
mechanisms, i.e., c¢ fi g and c fi g transformations. But,
at low temperature, another mechanism occurs. These results
will be published later. As shown in Fig. 7, the hardness resultsÕ
trend in this region is in agreement with region 2.
In region 4, according to Fig. 5, increasing the temperature
above 840 C causes the reduction of g volume fraction. Also,
the rate of increasing g volume fraction over time declines at
this region. As shown in Fig. 5 and 6(g) to (i), further
increasing the temperature leads to complete dissolution of the
g, so the microstructure is free of g at 900 C. Also, the
exothermic peaks of DTA at 930 C represent the g phase

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Fig. 6 SEM or optical microstructure of the alloy with different aging heat treatments: (a) and (b) 720 C; (c) 760 C; (d) 780 C; (e) 800 C;
(f) 820 C; (g) 840 C; (h) 860 C for 16 h; and (i) 900 C for 2 h
dissolution. According to Fig. 7, the hardness of the alloy at
this region declines as a result of c¢ dissolution. The g phase
reduces as well in the form of cellular or Widmanstätten.
The metallographic method was used to draw the time-
temperature-precipitation (TTP) diagram for the g phase.
Figure 9 is a TTP curve, which shows the initiation times and
temperatures of the precipitation of the g phase in different
morphologies. The left area of the C-shaped curve corresponds to
the g phase-free structures. However, increasing time and
temperature causes nucleation of Widmanstätten g into the grain
in addition to cellular g at the grain boundary. The g phase
formed after the precipitation of c¢ phase at the latter stage of
aging in the cellular mode and grew in a Widmanstätten
morphology into the grain. The amount of Widmanstätten g
Journal of Materials Engineering and Performance
phase also increased with aging time increase. This morphology
is shown in Fig. 4(b) and 6(h). As shown in Fig. 9, in the case of
A286, formation of cellular g at the grain boundary occurs at
temperatures lower than 840 C, while Widmanstätten morphol-
ogy of g is more obvious at the higher temperatures. This may be
explained considering a diffusive mechanism for growth of the
hexagonal g precipitates in the fcc matrix. At low temperatures
(between 650 and 840 C) where the matrix diffusion is slower
than the grain boundary diffusion, cellular g grows much faster
than Widmanstätten g. With increasing temperature, however,
matrix diffusion is accelerated and the Widmanstätten morphol-
ogy dominates. As reported by Asgari (Ref 22), diffusive growth
of the g plates occurs by the diffusion of solute to the incoherent
tip of g nuclei, resulting in the observed lengthening of g plates.
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Fig. 7 Variation of hardness with time and temperature of aging for solution-annealed A286 superalloy
As shown in Fig. 9, when the aging temperature is higher
than 760 C, the g phase starts to nucleate and precipitate at the
grain boundary after 8 h. It has been reported that many small
g precipitates are initially nucleated at the grain boundaries
during aging heat treatment, but only a few of them grow into
the matrix and coarsen to form the cellular morphology (Ref 7).
The precipitation peak temperature of the g phase is around
840 C. The C-type form of the TTP curve in Fig. 9 is the
result of the interaction between driving force and Ti diffusiv-
ity. However, at temperatures above 840 C, the g volume
fraction is decreased, but the Widmanstätten g phase increased.
It means that with increasing temperature, cellular g is reduced
and Widmanstätten g phase is formed.
According to the TTP curve in Fig. 9, further increasing the
temperature leads to complete dissolution of g in the matrix, so
the microstructure of the alloy is free of g at 900 C. The
saturation of solid solution at 860 C is low; therefore, the rate
of g formation is not sufficiently high and then the high rates of
diffusion at this temperature do not have further influence on g
precipitation. This indicates that the g phase is not a
thermodynamic equilibrium phase at that temperature and,
consequently, it transforms to c after prolonged aging.
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5. TTP curve of A286 superalloy for different morphologies

of g phase is drawn.

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