Transformation of η-phase into γ’-phase, γ-matrix and its effect on the high temperature

hardness and compression of Fe-Ni-based A286 heat-resistant superalloy

Muhammad Saqlain Qurashi1,*, Yajun Zhao1, Chuang Dong1, Lianchao Wang1,2 and Ying Li1,2
1 Department of Materials science, Dalian Jiaotong University, Dalian, 116028, P. R. China
2 Dongbei special steel group Co., Ltd. Dalian 116105, P. R. China
*Correspondent author

Abstract

Precipitation-hardening is achieved in an Fe-Ni-based A286 austenitic superalloy by means of

aging process. During the aging process gamma prime phases (γ’), eta (η) phases and TiC phases
nucleate in an austenitic matrix of this alloy. In this research, the behavior of η-phases’
precipitation, dissolution and transformation into γ’-phase and γ-matrix, and their consequent
effect on high temperature hardness testing and compression is investigated in an Fe-Ni-based
alloy. The behavior of phase nucleation is examined after aging at 710 ºC for different lengths of
time (1h, 2h, 4h and 8h). Scanning electron microscopy, adjacent with energy dispersive
spectroscopy (EDS) and transmission electron microscopy is used to identify the phases ((γ’)
Ni3(Al,Ti), eta (η) Ni3Ti and titanium carbides). The nucleation trend is declined with the increase
in time of aging and the 8h-aged sample is found to contain the lowest quantity of phases. Then,
the 8h-aged sample is investigated for η-phase’ dissolution and transformation behavior. Most of
the (η) Ni3Ti phases are transformed into gamma prime phases (γ’) Ni3(Al,Ti) because aluminum
is identified in dissolution areas. In (η) Ni3Ti phase dissolution areas, aluminum enhanced up-to
0.37wt.% which is more than double the amount used in composition and titanium increased up-
to 4.78wt.%, and nickel increases to more than 27.46 wt.%. Hardness range of the 8h-aged sample
is remained from 341 to 265 HV at each temperature from 50 ºC to 700 ºC respectively. Whereas
hardness range of 1h-aged sample was between 281 to 215 HV, which is almost 60HV lower than
the 8h-aged sample. During compression tests of the aged samples, it is found that the 8h-aged
sample showed almost negligible cracks in eta and TiC phases with deformation bands in austenitic
matrix. Here, synergic effect of deformation bands and γ’-precipitation enhanced the strengthening
of the 8h-aged sample.

Keywords: A286 superalloy; aging process; γ’, η and TiC phases; η transformation into γ’;
Hardiness and compression

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1. Introduction

Precipitation-strengthened superalloys like iron-nickel based A286 are widely-used in nuclear

reactors, aviation industry, aircraft, jet engines, and gas turbine industry [1-5]. Precipitation-
strengthening mechanism is achieved through an process of ageing heat treatment [2, 6]. In this
process, Fe-Ni based A286 alloy is aged above 700ºC for some time, after homogenizing and solid
solution heat treatment [2]. In the aging treatment gamma prime (γ’) Ni3(Al,Ti) phases are
nucleated in alloys which are coherent with its austenitic matrix [7,8]. Due to the coherency of the
crystal structure of gamma prime phases and austenitic matrix (FCC) in crystal structure, the
strengthening or hardening mechanism is enhanced [9-11]. However, finding the suitable
temperature and time which can give the maximum amount of γ’ phase, is a challenge. In the aging
process, three different kinds of phases nucleate in this alloy. These are fcc gamma prime (γ’)
Ni3(Al,Ti) phases, which are spherical in shape, hcp eta (η) Ni3Ti phases, which have a cellular
structure and fcc titanium carbides which are round or needle-like phases [1-13]. At high
temperatures from 600 ºC to 800 ºC, γ’ phases transform mostly into eta hcp eta (η) Ni3Ti phases
which degrade this alloy’s performance [12-16]. Eta phases nucleate only on grain boundaries,
whereas the other two nucleate throughout the austenitic matrix of this alloy [17]. The precipitation
and dissolution behavior of these phases in A286 superalloy is an important area of research in
order to achieve excellent mechanical properties.

Precipitation and dissolution or transformation into other phases can occur at any time during hot
working, this highly depends on the temperature, time and composition of the alloy. Many
researchers found that the volume fraction curve of η and γ' phases fluctuates a lot in the
temperature range of 600 ºC to 750 ºC [2,6,18,19]. M. Savoie et al. [20] found that the size of γ'
precipitate distribution in alloy A-286 is higher when it is aged at 720 ºC for 16h. Seifollahi et al.
[18] stated that the volume fraction of both η and γ' phases are highly dependent on the Ti/Al ratio
in the composition of A286 when it is aged between 600-800°C for different periods of time.
Therefore, there is the possibility of a higher dissolution of eta phases rather than precipitations
around 700 ºC for specific times of aging. Generally, it is accepted that if the time and temperature
increase, γ' precipitate distributed throughout the matrix decreases and η precipitate nucleation
increases around the grain boundaries [21-24]. But it is important to find the ideal temperature and
time when the nucleation of γ' phases are highest and the formation of η phases are lowest.

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Some researchers found that η phases affect the strengthening mechanism positively [25, 26] but
most stated that η phases are responsible for brittleness, crack initiation and degradation of creep
behavior in an iron-nickel based A286 alloy [4,6,10,11,27]. Strengthening by γ' in A286 is widely
acclaimed by many researchers [2-7] but other phases like TiC could have a great impact in Fe-Ni
alloys, however, this has not been studied thoroughly. TiC ceramic-particles are considered to be
the reinforcement elements in the strengthening mechanism [28-30], same as gamma prime phases.
But the size of gamma prime phases are much smaller (2nm~65nm when aged from 680 ~780 ºC
for different lengths of time) [4,18, 20, 31] than the TiC phases (mostly from 1µm to 5um) [32].
The size, shape and distribution of TiC have a significant effect on mechanical properties. TiC
phases’ small size and homogeneous distribution add value to the mechanical performance of the
alloy. A bigger size and uneven distribution of both eta and TiC cause brittleness and crack
initiation sites during hot-working [28, 29]. Ti is the common constituent of the above mentioned
phases, so it’s composition in A286 alloys will have a definite effect on strengthening. During
compression or deformation, these phases can cause crack initiation. Additionally,
deformation/dislocation bands and gamma prime phases (γ') can hinder the crack propagation and
enhance the strengthening mechanism [33-36].

As inferred, in an iron-nickel based A286 superalloy, these phases nucleate, dissolve or

transformed during the aging process. Dissolution of gamma prime phases has been studied in
depth but the dissolution of eta phases and their transformation into gamma prime phases has not
been studied in much detail. In this research, the A286 superalloy was designed under aerospace
materials specification (AMS) standard parameters. Through the aging process it is studied how
eta phases transform into gamma prime phases or dissolve into austenitic matrix due to the effect
of aging time, which ultimately results in precipitate hardening. Using the aging treatment
technique for different periods of time, the precipitation, dissolution and transformation behavior
of η into γ' and γ phases was examined. Thus, it is possible to analyze how this phenomenon
influences the hardness at higher temperatures and the compression strength of this alloy.

2. Material selection and experimental

The examined iron-nickel based alloy is composed of 54Fe-25Ni-15Cr with small amount of other
elements as can be seen in Table 1. The composition of this alloy was designed according to the
elemental range of aerospace material specifications (AMS) of an A286 superalloy i.e., Carbon

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0.08 max, Manganese 2 max, Silicon 1 max, Phosphorous 0.025 max, Sulfur 0.025 max,
Chromium 13.5-16, Nickel 24-27, Titanium 1.9-2.6, Vanadium 0.10-0.50, Aluminum 0.35 max,
Boron 0.0003-0.010, Cobalt 1 max and copper 0.35 max and molybdenum 1-1.5 [2].

Table 1. Chemical composition of Fe-Ni based A286 superalloy.

Sample Ni Cr Fe Mn Co Cu Mo V Al Ti Si C
24.95 14.93 53.96 1.21 0.33 0.35 1.06 0.28 0.15 2.58 0.16 0.05

This alloy is produced in a laboratory by a non-consumable arc melting furnace where high
temperatures are generated by arc discharge in order to melt the raw materials in the water-cooled
copper crucible, under the protection of the inert gas argon. In order to homogenize the alloy
components in the raw materials during melting, a manual stirrer was used to flip the ingot. An
ingot of 50 grams was arc-melted using 99.99% pure elements, as shown in Table 1. For
metallographic purposes, the cast ingot was cut into square test coupons with dimensions of 8×8×3
mm using a water cooled wire cutting machine. These test coupons or specimens were first
homogenized at 1180°C for 5 hours, followed by water quenching. Then, these specimens were
exposed to solid solution heat treatment 990°C for 2h and subsequently water quenched. After
homogenizing and solid solution heat treatment, an X-ray diffractometer (EMPTREAN-XRD with
Co Kα radiation (λ = 1.789Å) at the scanning rate of 4°/min from 30° to 150°) was used to
characterize the crystal structures of the newly-made alloy. For that purpose, samples were
polished with 280~2000-grit SiC emery-papers. For aging treatment, the temperature was set at
710°C for 1, 2, 4 and 8 hours with air quenching. After aging, samples were used for microstructure
analysis. Prior to analysis, samples were first ground mechanically using 280~3000-grit SiC
emery-papers. After obtaining a smooth scratch-free surface by grinding with the finest emery-
papers, samples were polished with polishing machines to achieve a mirror-like surface. Then,
these prepared samples were immersed into a chemical etchant (70 v% H2O + 20 v% HF + 10 v%
HNO3) for about one minute to reveal microstructures on the polished surfaces. Optical
microscopy (OM; Leica DMi8 A) was done after each aging treatment to check the effect of the
lengths of time on nucleation. Nucleated phases were further identified using a scanning electron
microscope (SEM-Supra 55) equipped with an energy dispersive spectrometer (EDS). Line scan
and point scan EDS was done on many point of the surface to examine the phase compositions.

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Image pro-plus (IPP) software was used for quantitative analysis of the phases on SEM and OM
image of different magnifications. For further identification of phases, transmission electron
microscopy (TEM) was needed, because it can generate a highly-magnified image, measured in
nanometers. So for TEM purposes, samples were mechanically thinned up-to a thickness below
80µm, then again further thinned to nano scale using a precise ion polishing system (Gatan, PIPS
II 695, 6–3 keV and ±8.5°~±2.5° in a vacuum). Then samples were exposed to a transmission
electron microscope (TEM: JEOL, JEM-2100F) and selected area diffraction pattern (SADP).

For high temperature hardness (Vickers micro-hardness testing machine: Model-ZD-HVZHT-30)

measurements, the same samples were used and were examined for microstructure analysis after
aging. Indentations dwelled for 15 seconds by load of 2000 g. For compression tests samples were
directly cut from an ingot in square dimensions of 3×3×6mm. Then, these samples went under the
same heat treatment procedure of aging, as done for the microstructure analysis. Compression tests
were conducted at room temperature (30% compressed) using a universal testing machine (UTM
5105 electronic universal tester-50 Ton) at the strain rate of 0.5 mm/min.

3. Results and discussion

Iron-nickel-based alloy A286 was used after aging treatment, because after aging gamma prime
phases and titanium carbides have nucleated which have a beneficial effect on the strengthening
mechanism of the alloy. It is a reason that this alloy is typically called precipitate-hardened alloy
[1-6]. Before aging, samples went under homogenization and solid solution treatment. The XRD
pattern in figure 1 shows that up until this point only a single austenitic phase had appeared.

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 After homogenizing
After homogenizing+solid solution


Intensity / a.u.




20 30 40 50 60 70 80 90 100

2
Figure 1. XRD pattern of the heat-treated sample of iron-nickel based A286 superalloy before
aging

3.1 Evolution of phases after aging treatment

In figure 2 microstructures of the aged specimens can be seen. Those were treated at the same
temperature of 710 ºC but for a different lengths of time. Two different kinds of optically-visible
phases appeared in the austenitic matrix of all samples, as other researchers observed [23, 24].
There should also be gamma prime phases, whose size is comparatively very small [4,18, 20, 31].
For examining gamma prime phases, TEM analysis was done which is shown in figure 3.

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 Figure 2. Optical Microstructures (OM) of A286 superalloy after aging at 710 ºC for different
lengths of time (a) 1h (b) 2h (c) 4h (d) 8h

Identification of these phases was done by SEM-EDS and dark-field TEM as shown in figure 3
and 4. In the SEM image (figure 3(a)), it is obvious that there are three different phases. TEM and
SADP pattern showed that these are gamma prime (γ’) Ni3(Al,Ti), eta (η) Ni3Ti and titanium
carbides. Figure 3(b) is a TEM image of TiC with SADP along the [011] zone axis. Titanium
carbides grew in a face-centered cubic structure, space group Fm3m and lattice parameter α=4.32Å.
This phase, ovoid shaped or plate-like, is often observed at grain boundaries and within grains [28,
29, 37], as can be seen in figure 2(a, d). Figure 3(c) is the TEM of eta phase (Ni3Ti) with SADP
pattern along [2-1-10] zone axis which is hcp structure. From the cellular shape of the η-phase, it
is anticipated that there is high lattice misfits between the austenitic matrix and the η-phase, which
is caused by the aging process [38]. The formation of the η-phase in A286 is known to occur during
the aging process or hot working. Investigations report that the η-phase often precipitates in the
form of Widmanstatten or cellular particles at the grain boundaries [6, 7, 12]. Figure 3(d) shows

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the dark-field TEM image, where nanometer-sized precipitates are distributed throughout the
microstructure. These are shaped like round spheroids and are clearer in SEM (figure 3(a)), shown
with red arrows. In the selected area diffraction pattern along the [001] zone axis, as shown in
SADP of figure 3(d), clear {200} and {220} reflections of the austenitic matrix are visible, as well
as {100}, {110}, {111} and {120} superlattice reflections of the precipitation with an ordered fcc
structure. These are characteristic of the gamma prime phases (γ'-Ni3(Al, Ti)). Aging heat
treatment of this alloy let to formation of this (γ') hardening phase. The interesting strengthening
properties of the A286 alloy are due to this phase acting by microscopic mechanism [2-6], which
is related to interactions between mobile dislocations and precipitates [37]. The γ' phase
crystallizes in a cubic structure (space group Pm-3m) with a lattice parameter α=3.57 Å. This phase
is coherent with an austenitic phase γ matrix (Fm3m α=3.60 Å).

Figure 3. Phase identification of A286 alloy after aging treatment at 710 ºC (a) SEM of aged
sample (b) TEM and SADP of TiC phase (c) TEM and SADP of eta (η) phase (d) TEM and
SADP of gamma prime phase (γ')

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After aging, a fourth kind of phase was also found, but in an amount negligible quantity. Figure
4(a) shows the SEM of phase in which a dark black phase was surrounded by a dark grey phase.
Line EDS on this point (figure 4(b)) was done to identify its composition. It is found that it is
TiC(Al2O3). Studies tell us that there could be Ti(C, N) or Ti compound with W [15, 37] also, but
in this research the presence of these elements was not significantly found.

Figure 4. Phase identification of A286 alloy after aging treatment at 710 ºC (a) SEM of aged
sample (b) SEM-EDS of TiC(Al2O3) phase

From figure 2, it can be observed how these phases nucleated in the austenitic matrix of A286
alloy. Eta (η) phases have only grown on the grain boundaries and TiC have been observed
throughout the matrix. From figure 2((a)1-hour aged) to 2((d) 8-hour aged) there seems to be some
dissolution as the time of aging increases. Or in other words, at the aging time of 8 hours at 710
ºC, a lower amount of eta and TiC phases were exhibited, as shown in figure 2(d). Many
researchers found that eta phases start generating from 600 ºC to 850 ºC and there can be rise and
fall of generation curves [4,6,18,20]. So, here this alloy showed less generation of phases when
aged at 710 ºC for 8 hours. Therefore, this temperature (710 ºC) and these times (1,2,4 and 8 hours)
are ideal for studying the phenomenon of eta phase dissolution and, more importantly, how these
eta phases dissolve. In addition, whether they transform into gamma prime phases or whether they
transform into austenitic phases and how they ultimately affect the strengthening mechanism.

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 200
1h aged 1h aged
2h aged 2h aged
20
4h aged 4h aged
8h aged 8h aged
150

Probability
Probability

15

100
10

50
5

0 0
0.0 0.5 1.0 1.5 2.0 2.5 3.0 0 5 10 15 20 25

TiC size (m) Eta phase size (m)

Figure 5. Statistical analysis of eta phases and TiC phase formed in A286 aged alloys

Statistical analysis of TiC and Eta phases showed the trend of generation with respect to time on
the same aging temperature. When samples were aged for 1 hour, TiC phases were significantly
nucleated compared to the samples aged for longer times. The maximum size at this stage was up-
to 2.7µm. The lowest probability of TiC existence was found when samples were aged for 2 hours
with the maximum size of 2 µm. When samples were aged at 8 hours, TiC phase size was decreased
slightly to 2 µm but the probability of formation was increased and the maximum quantity of TiC
was found between 0.25 to 0.5 µm. This behavior of existence of TiC species can also be observed
in figure 2. With regard to eta phases, maximum eta phases were nucleated in the sample which
was aged for 2 hours with the maximum size of 25 µm. The maximum probability of existence of
eta phases was in the size range of 8 µm. However, when samples were aged for 8 hours, fewer
eta phases were formed, which can also be seen in figure 2. Bigger eta phases were found dissolved
into the austenitic matrix or into the gamma prime phases in the 8h-aged A286. How these phases
dissolved or transformed into γ-matrix or γ'-phase is described in the next section. Formation
behavior of these phases has notable effect on strengthening mechanism [23, 24, 28, 29].

Quantitative analysis of the gamma prime phase was not done in this research, because of their
very small sizes and to avoid the overlapping of very small γ'-particles which could also fade into
austenitic matrix [39-41].

3.2 η-phase (Ni3Ti) transformation into γ'-phase (Ni3(Al, Ti) and γ-matrix

Figure 6 shows the pattern of transformation of η-phase (Ni3Ti) when samples were aged for 8
hours. Figure 6 (a) is an optical microscopic image. Yellow arrows point to the area where eta

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phases have been diminished and seem to be faded into the austenite matrix. In the next SEM
image of this figure (6 (b)), the disappearance of the eta phases is more apparent. Transformation
has occurred from the grain boundary to the end of phase. In order to examine the transformation
of η-phase (Ni3Ti), a higher magnification was used, as can be seen in figure 6(c). Here it is clear
that η-phases are transforming into γ'-phases. Conversion of lamellar structure into small round
spheroid phases are clearly visible in figure 6(c). These round phases are γ'-phases, which can also
be seen all around the austenitic matrix of this figure 6(c). Figure 7 shows that SEM with point
scan EDS of eta phase area of the 8h aged sample in various places. It can be seen that the shape
of the phase is changing into spheroids and it is vanishing into the γ-matrix. The amount of
aluminum has increased in spheroid structure, which means it has transformed from η-(Ni3Ti) to
γ'-(Ni3(Al, Ti). In figure 6(d), a complete transformation of η into γ-matrix can be seen. Therefore,
it can be conclude that eta firstly transformed into gamma prime phases, before its complete
dissolution into the γ-matrix.

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 Figure 6. Magnified images of A286 aged for 8h, showing the dissolution behavior: (a) Optical
micrograph (b) SEM of dissolving eta (c) dissolution of eta (η) into gamma prime phases (γ’) (d)
dissolution of eta into austenitic matrix

Below in figure 7, there is a highly-magnified SEM image of dissolved areas of η-phases in the 8-
hours aged sample. In SEM-EDS figure 7, it is clear that the EDS point area in figure 7(c, d)
contains a higher amount of aluminum, titanium and nickel (shown by red markings) which are
the constituent elements of gamma prime phase [γ'- (Ni3(Al, Ti)]. SEM-EDS point area as shown
in figure 7(a, b) is austenite, which means here at this point eta has completely dissolved into the
austenite (γ) matrix. In EDS point area of figure 7(d) aluminum increased from the alloy’s
constituent 0.15wt.% to 0.37wt.% in this γ' phase, which is more than double the amount and
titanium increased from 2.58wt.% to 4.78wt.%, and nickel increased from 24.95wt.% to
27.46wt.%.

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Figure 7. SEM image of 8h aged sample (a) SEM-EDS point showing complete dissolution of η-
phase into γ-matrix (b) SEM-EDS point showing dissolution of η into γ’-phase (e) SEM-EDS of
eta phase

In figure 8, an SEM line EDS was done on the area of the eta phase structural transformation. In
such places in SEM observations of the 8h-aged sample, it was found that cellular structures were
becoming spheroidal. Line EDS was done to check which element was entrapping there. Line EDS
evidence (figure 8(b)) showed that aluminum (Al) was increasing into eta phase constituents (Ni3Ti)
which is gamma prime phase’s constituents (Ni3(Al, Ti).

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 Figure 8. SEM image of 8h aged sample (a) formation of gamma prime spheroids into cellular
eta structure (b) line scan EDS Aluminum increment into eta phase

This kind of phenomenon, the lamellar structure is transforming into spheroids has also been
observed by other researchers, but in different alloys [42, 43]. Eta phases on the grain boundaries
in figure 8(a) can be seen. Some eta phases have fully disappeared, some are vanishing, and some
are turning into round spheroids where the scan line of EDS was done. In many places in the 8h
aged sample’s microstructures, eta phases can be seen transforming into gamma prime phases.

3.3 Effect of η-phase (Ni3Ti) transformation on mechanical performance

Hardness and compression tests were carried out because in this kinds of analysis, precipitations
and deformation directly affect the strengthening mechanism. Figure 9 shows the hardness of A286
samples, which were aged for 1, 2, 4 and 8 hours. From 50 ºC to 700 ºC, on each spot, three test
of hardness were taken on already aged samples. The trend of hardness decreases with the increase
of temperature. Many researchers achieved the same results, that is, with the increase of
temperature, hardness decreased [17, 39]. However, as the time of aging increases, hardness also
increases. The 8h-aged samples showed significantly higher hardness at each temperature.
Hardness range of 8h aged sample remained from 341 HV to 265 HV whereas hardness range of

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1h aged sample was between 281 (highest) to 215 HV, which is almost 50HV lower than the 8h-
aged sample.

340

320
1h
Vickers Hardness (HV) 2h
4h
300
8h
280

260

240

220

0 100 200 300 400 500 600 700

Temperature (C)
Figure 9. High temperature hardness curves of aged alloys with different time

Figure 10 shows the microstructure of the top surface when all aged samples were compressed up-
to 30% at room temperature. SEM Microstructures are shown here with their magnified images to
observe clearly how compression has affected on the samples. The compressed sample which was
aged for one hour, contains crack sites, not only on TiC phases, but also on the deformation bands
or dislocation points, which can be seen in figure 10 (a, b) with a magnified image. TiC cracks are
indicated by yellow arrows and eta cracks are indicated by purple arrows, and deformation bands
are shown with black dotted lines. When the sample was aged for 2 hours (figure 10 (c, d)), fewer
deformation bands were found, but TiC phase and also eta phases both were displayed cracked.
Deformation/dislocation does not bring structural strength here, which leads to cracks in phases.
When samples were aged for 4 hours (figure 10 (e, f)) and compressed, the same phenomena as in
2-hour aged sample were found but in smaller quantity. The sample with 8-hour aging (figure 10
(g, h)), showed the lowest, almost negligible amount of cracks. However, many deformation bands
were found.

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Figure 10. SEM micrograph of A286 samples after 30% compression (a, b) 1h aged sample (c, d)
2h aged sample (e, f) 4h aged sample (g, h) 8h aged sample
Figure 11 is the magnified SEM image of the 2-hours aged and the 8-hours aged samples after
compression. The 2h-aged sample was observed with the maximum amount of eta phases and the
8-hours aged sample observed with the lowest amount of eta phases. 2-hours aged and 8-hours
aged samples can be compared in figure 11. Figure 11 (a) has few gamma prime phases with some
deformations/dislocations. Figure 11 (b) is of the 8h-aged sample, which has more
deformations/dislocations and is also full of gamma prime phases.

Figure 11. Magnified SEM images after compression: Existence of γ'-gamma prime phases (a)
2h aged sample (b) 8 hour aged

The synergy of deformations/dislocations and gamma precipitates has reinforced the strengthening
mechanism, as precipitates impede the dislocations which serves to harden the material [33, 34] as
is observed during compression (figure 10) and high temperature hardening tests (figure 9).
Therefore, it is stated by the researchers that the interesting strengthening properties of the A286
alloy are due to this gamma phase acting by microscopic mechanisms, such as the Orowan
mechanism [35], which is related to interactions between mobile dislocations and precipitations
[37]. L. Fournier et al. [36] discussed the influence of deformation due to cycle fatigue on this
precipitation-strengthened A286 austenitic stainless steel and found that the fatigued A-286 (in our
case compressed) went into strain hardening if there are no gamma precipitate-free localized
deformation dislocations. Moreover, it was demonstrated that the presence of γ' precipitates-free
localized deformation bands correlates strongly with the stress corrosion cracking susceptibility of
A286. Moreover, it was clearly demonstrated that the specimens not containing γ' precipitate-free

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localized deformation exhibit little or no crack susceptibility. Therefore, it can be concluded in
this research that the 8-hour aged sample showed less crack susceptibility with dislocations
because of the existence of a high quantity of gamma prime (γ') precipitations, as can be seen in
figure 10. Deformations or dislocation itself cause hardening or strengthening when force is being
applied. This means that the presence of higher dislocation bands can have higher induced
strengthening due to shearing mechanism of precipitates (gamma prime phases) [36, 44]. Due to
this impediment of higher gamma prime phases and deformation bands during deforming, the 8h
aged sample showed maximum hardness, even at higher temperatures.

4. Conclusion

The objective of this work was to investigate the behavior of η-phase (Ni3Ti) transformation into
γ'-phase (Ni3(Al, Ti) and γ-matrix, and their subsequent effect on strengthening mechanism in iron-
nickel-based A286 precipitation-strengthened superlloy, after aging at 710ºC for different lengths
of time. High temperature hardness and compression tests were conducted to analyze the effect of
phases’ precipitations, dissolution and transformation effect.

1. After aging the samples at 710 ºC for different lengths of time (1h, 2h, 4h and 8h), OM,
SEM, EDS and dark-field TEM analysis were conducted. Three kinds of precipitate
nucleated in this alloy, these are η-phase (Ni3Ti), γ'-phase (Ni3(Al, Ti) and titanium
carbides species. The 2h-aged samples showed the maximum amount of η and TiC and the
trend of nucleation fell as the aging time increased. The 8h-aged sample showed the lowest
amount of η and TiC phase. In SEM-EDS analysis of the 8h-aged sample, it was found that
there eta phases were significantly transformed into γ'-phase (Ni3(Al, Ti) and some eta
phases were completely dissolved into the austenitic matrix.
2. The 8h aged sample showed the maximum hardness at each temperature level from 50 ºC
to 700 ºC. The 1h aged sample revealed from 281 HV at 50 ºC to 215 HV at 700 ºC.
Whereas the 8h aged showed from 341 HV at 50 ºC and 265 HV at 700 ºC. The reason for
this is that the 8h-aged sample was found with a minimum amount of eta (η) phases and a
maximum amount of gamma prime phases (γ').
3. 30% compression showed that 1h, 2h and 4h aged samples were found with eta phase
cracks, TiC cracks and with a minimum amount of deformation bands. Compared to the 1,
2, 4h-aged samples, the 8h-aged sample contained no cracks, but full of deformation bands.

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 In magnified SEM image analysis after compression, it is found that the 8h-aged sample
was full of gamma prime phases. The synergic effect of gamma prime phases (γ') and
deformation bands enhanced the strengthening mechanism during deformation
(compression or hardness tests).

Acknowledgements

The present work was financially supported by the Key Discipline and Major Project of Dalian
Science and Technology Innovation Foundation (Grant No. 2020JJ25CY004), and Project
supported by Scientific Research Fund of Liaoning Provincial Education Department: (Grant No.
JDL2020014), and supported by Shunde District Science and Technology Project (Grant No.
201911220001)

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