Journal of Materials Science & Technology 67 (2021) 95–104

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Invited Review

Precipitate coarsening and its effects on the hot deformation behavior

of the recently developed ␥’-strengthened superalloys
Yuting Wu a , Chong Li a,∗ , Xingchuan Xia b , Hongyan Liang a , Qiqi Qi a , Yongchang Liu a,∗
a
State Key Lab of Hydraulic Engineering Simulation and Safety, School of Materials Science & Engineering, Tianjin University, Tianjin, 300354, China
b
School of Material Science and Engineering, Hebei University of Technology, Tianjin, 300130, China

a r t i c l e i n f o a b s t r a c t

Article history: Recently, the ␥ -strengthened superalloys are of great interests in high temperature applications due to
Received 22 March 2020 their excellent high temperature strength which is derived from the ␥ strengthening phase. For these
Received in revised form 23 May 2020 ␥ -strengthened superalloys, the changes in morphology, size and distribution of ␥ precipitates due to
Accepted 2 June 2020
coarsening during thermal exposure have a significant impact on the properties of alloys. This article
Available online 21 July 2020
briefly summarizes the recent advances on the coarsening behavior of gamma prime precipitates in
the recently-developed ␥ -strengthened superalloys and its effects on the hot deformation behavior of
Keywords:
superalloys, drawing specific examples on Allvac® 718PlusTM and Ni3 Al-based intermetallic superalloys.
␥ -strengthened superalloy
Microstructure
It is found that the particle size plays an important role in morphological evolution of ␥ precipitates. For
Coarsening instance, the morphology of ␥’ precipitates evolves from cuboidal to strip-like or other complex structures
Hot deformation in Ni3Al-based intermetallic alloys, while the ␥’ precipitates in Allvac® 718Plus alloy always present near-
spherical morphology due to the relatively small initial particle size. The Lifshitz-Slyozof-Wagner (LSW)
theory and its modifications, as well as Trans-Interface Diffusion Controlled (TIDC) theory have been
applied to describing the coarsening kinetics of ␥’ precipitates. Additionally, the hot deformation behavior
of ␥ -strengthened superalloy is found to be greatly influenced by the coarsening of ␥ precipitates.
© 2021 Published by Elsevier Ltd on behalf of The editorial office of Journal of Materials Science &
Technology.

Contents

1. Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 96
2. Microstructural characteristics of the typical ␥’-strengthened superalloys . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 96
2.1. Ni3 Al-based intermetallic alloys . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 96
2.2. Allvac 718PlusTM superalloy . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 97
3. Coarsening behavior of the ␥’ precipitate . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 98
3.1. Morphological evolution of the ␥’ precipitates . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 99
3.2. Coarsening kinetics of the ␥’ precipitates . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 100
4. Hot deformation behavior of ␥’-strengthened superalloys . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 101
4.1. Hot deformation behavior . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 101
4.2. Effects of the ␥’ precipitates coarsening on hot deformation behavior . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 103
5. Concluding remarks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 103
Acknowledgements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 104
References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 104

∗ Corresponding authors.
E-mail addresses: lichongme@tju.edu.cn (C. Li), ycliu@tju.edu.cn (Y. Liu).

https://doi.org/10.1016/j.jmst.2020.06.025
1005-0302/© 2021 Published by Elsevier Ltd on behalf of The editorial office of Journal of Materials Science & Technology.
Y. Wu et al. Journal of Materials Science & Technology 67 (2021) 95–104

1. Introduction

Owing to the good mechanical properties and corrosion resis-

tance at elevated temperature, nickel-based superalloys have
attracted extensive attention for its widespread applications in air-
craft and power-generation industry over past few decades [1–6].
According to the statistics, Ni-based superalloys are by far the
most used high-temperature structural material in advanced aero-
engines, accounting for more than 40 % of the total weight. Ni-based
superalloys are a class of precipitation-strengthened superalloys,
and its superior properties are derived from the strengthening
precipitates. Variations of alloying elements have introduced two
different main strengthening precipitates in Ni-based superalloys, Fig. 1. The crystallographic prototype structure of the ␥ precipitate, revealing a
face-centered cubic L12 crystal structure.
known as ␥ (chemical composition of Ni3 Al) and ␥ (chemical com-
position of Ni3 Nb) [7–10]. Most of the precipitation-strengthened
Ni-based alloys are principally strengthened by the ␥ precipitates
which present an ordered L12 crystal structure, as displayed in
Fig. 1. In some Ni-based superalloys, such as Inconel 718 (hereafter
referred to as IN718) and Inconel 625 alloy, ␥ precipitates with
a DO22 crystal structure are the predominant strengthening pre-
cipitates and its crystallographic prototype structure is presented
in Fig. 2. In addition, a few Ni-based superalloys are strengthened
by both ␥ and ␥ precipitates, such as Inconel 706. However, the
␥ precipitate is thermodynamically unstable at relatively high
temperature. Taking the IN718 alloy as an example, the stability
of ␥ precipitates leads to that the upper working temperature
of this alloy is limited to 650 ◦ C. During the prolonged expo-
sure at above 650 ◦ C, the metastable ␥ precipitate transforms to
ıphase with orthorhombic structure, resulting in the correspond-
ing deteriorations of strength and service life [11]. According to a
multitude of experiments and researches, the Ni-based superalloys
strengthened by ␥ precipitates present improved high tempera-
ture capability than those strengthened by ␥ precipitates due to
the higher thermal stability of ␥ precipitates over ␥ precipitates Fig. 2. The crystallographic prototype structure of the ␥  precipitate, displaying a
body-centered tetragonal DO22 crystal structure.
[12,13].
It is a thermodynamic truism that an engine (whether in power-
generation industry or aircraft engine industry) possesses higher alloys and Allvac 718Plus superalloy are the subject of numerous
efficiency at higher operating temperature [14]. In modern aircraft researches.
engines, both the thrust-to-weight ratio and the working temper-
ature of the combustion chamber increase continuously, which 2.1. Ni3 Al-based intermetallic alloys
leads to the urgent requirements of novel high-performance mate-
rials with improved high-temperature capability and mechanical Compared with conventional alloys, intermetallics possess rel-
properties. As mentioned above, the higher thermal stability of atively high melting point and high strength at high temperature
␥ precipitates has suggested the demand of the development of owing to its long-range ordered (LRO) structure [19–23]. Since the
␥ -strengthened superalloys. In this work, the coarsening behavior ␥ phase in nickel-based alloys was firstly researched at 1940s, it
of ␥ precipitates and corresponding coarsening mechanism in ␥ - is one of the disquisitive hotspots in which the researchers are
strengthened superalloys during thermal exposure are reviewed. interested [19]. It is exactly based on the unique properties of ␥
Furthermore, the effects of ␥ precipitates coarsening on the hot phase that Ni3 Al-based intermetallic alloys with high ␥ volume
deformation behavior of alloys are also discovered. fraction have attracted considerable attention over past decades.
The Ni3 Al-based intermetallic alloys have excellent physical and
mechanical properties, especially in the field of high temperature
2. Microstructural characteristics of the typical properties, such as high strength and creep resistance, excellent
␥’-strengthened superalloys corrosion resistance and relatively low density etc. [24,25]. How-
ever, the polycrystalline Ni3 Al-based alloys are easily inclined to
To meet the requirements for the alloys with improved per- intergranular cracking because of its extremely poor room tem-
formance for the early jet engines, the earliest superalloy, i.e. perature ductility, which leads to the fact that the research of
Nimonics were developed by the Mond Nickel Company (now Ni3 Al-based alloys once almost remains stagnant. Aoki and Izumi
INCO) in 1940s [15]. The ␥ (Ni3 Al) phase has proven to be closely [26] found that microalloying with trace boron (∼ 0.4 wt.%) in
related to the strength of superalloys. Hence, since the advent of Ni3 Al-based intermetallic alloys helps to dramatically improve the
the first superalloys, much attempts have been made to improve ductility. Following this finding, extensive researches have been
high temperature capability and processability of ␥ -strengthened conducted on the microstructures and properties of Ni3 Al-based
superalloys. Accordingly, the operating temperature of current ␥ - alloys with various alloying addition. As a consequence, a num-
strengthened superalloys is increased to above 1100 ◦ C. Fig. 3 ber of Ni3 Al-based alloys with strictly designed compositions were
lists the grades and the year of introduction of some commer- developed for commercial application over past few decades. The
cial ␥ -strengthened superalloy. Among the novel superalloys with chemical compositions of some commercial Ni3 Al-based alloys are
enhanced high temperature properties, Ni3 Al-based intermetallic listed in Table 1.

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Y. Wu et al. Journal of Materials Science & Technology 67 (2021) 95–104

Fig. 3. Development of some ␥ -strengthened superalloys [15–19].

Table 1
Chemical compositions of some typical Ni3 Al-based alloys for commercial applications [19,27,28].

Alloy Al Cr Mo Zr W Ti Fe Hf B C Ni

IC-50 11.30 – – 0.60 – – – – 0.02 – Bal.

IC-221 8.50 7.80 – 1.70 – – – – 0.02 – Bal.
IC-396 7.98 7.72 3.02 0.83 – – – – 0.005 – Bal.
IC-396LZr 7.98 7.72 3.02 0.20 – – – – 0.005 – Bal.
IC6 7.5−8.5 – 10−14 – – – – – ≤0.15 – Bal.
VKNA-1V 8.83 5.58 3.50 0.45 2.82 1.54 – – – 0.03 Bal.
MX246 7.0−8.5 7.4−8.2 – 0.3−0.8 – 0.6−1.2 ≤2.0 – 0.01−0.05 0.06−1.16 Bal.
MX246A 7.6−8.5 7.4−8.2 3.5−4.5 – 1.7−2.3 0.6−1.2 ≤2.0 0.2−0.6 0.01−0.05 0.06−0.2 Bal.

Fig. 4. The microstructures of a newly designed as-cast Ni3 Al-based alloy, revealing a dendrite structure: (a) optical image; (b) SEM image.

Our previous works [29] have investigated the microstructure of
an as-cast Ni3 Al-base alloy which is introduced on the basis of the
IC396 series Ni3 Al-based alloy by adjusting the alloying elements.
Small amount of Fe element is added to improve the weldability of
the alloy. Fig. 4 represents the microstructure of a Ni3 Al-base super-
alloy, revealing that the microstructure mainly consists of dendritic
␥+␥’ phases (light areas in Fig. 4(a)) and interdendritic phases (dark
areas in Fig. 4(a)). In ␥+␥’ dendrites, the cuboidal ␥’ precipitates
with an ordered L12 structure embedded in the continuous disor-
dered ␥ phase with face centered cubic (FCC) structure. It also can
be observed that some nanometer ␥’ particles precipitated in the ␥
channels, as indicated by yellow dotted circle in Fig. 4(b). Besides of
the ␥’ phase and ␥ phase, ␤ phase with B2 structure, ␣-Cr precipi-
tate and some kind of carbides (such as HfC, TiC etc.) also precipitate
in Ni3 Al-based intermetallic alloys with various alloying additions
[24,30–32].
It is known that the microstructure characteristics of alloys,
including phases, morphology, size and distribution, are consider-
ably related to the alloying elements. Liu et al. [33] demonstrated
that the sufficient addition of Fe element promotes the precip-
itation of ␤ phase in Ni3 Al-based alloy and the stability of ␤
phase is very sensitive to Al-Ni ratio. Zhang et al. [28] studied the
microstructure of MX246 and MX246A alloy, and further clarified
the effect of alloying elements on the microstructure. They found
that the microstructure of MX246 and MX246A alloy is mainly com-
posed of dendrite ␥+␥’ and eutectic ␥-␥’. Both the amount and size
of ␥-␥’ eutectic phase decreased with the addition of Mo and Hf,
and the stability of ␥’ precipitates increased. The investigation per-
formed by Li et al. [34] shown that the volume fraction, size and
cubical degree of ␥’ phase in the Ni3 Al based single crystal alloys
increased with the addition of Ta.
2.2. Allvac 718PlusTM superalloy
IN718 alloy has been widely used for high temperature
applications in the last few decades due to its advantages of
high temperature strength, good workability and moderate cost
[35–37]. However, as the main strengthening phase in IN718 alloy,
metastable ␥” phase transforms to ı phase during prolonged expo-
sure at above 650 ◦ C, which leads to the deterioration of strength
and service life. Consequently, IN718 alloy can only be applied at
the temperature below 650 ◦ C. Waspaloy alloy which is princi-

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Y. Wu et al. Journal of Materials Science & Technology 67 (2021) 95–104

Fig. 5. The microstructures of 718Plus alloy supplied in the form of a forged gas turbine disc: (a) SEM image indicating ␩ phase and carbides; (b) TEM image.

Table 2
A comparison in the chemical composition of Waspaloy alloy, 718 alloy and 718Plus alloy [18].

Alloy Cr Fe Al Ti Mo W Co Nb C P B Ni

Waspaloy 19.4 – 1.3 3.0 4.25 – 13.25 – 0.035 0.006 0.006 Bal.
IN718 18.1 18 0.45 1.0 2.8 – – 5.4 0.025 0.007 0.004 Bal.
718Plus 18.0 10 1.45 0.7 2.75 1 9 5.45 0.02 0.014 0.004 Bal.

pally strengthened by ␥’ phase exhibits about 60 ◦ C higher working

temperature compared to IN718 alloy, but its applications are
restricted by the poor workability, weldability and relatively high
cost. To overcome these deficiencies, a new Ni-based alloy was
introduced by ATI Allvac, designated as Allvac 718PlusTM alloy
(hereafter referred to as 718Plus) [18]. 718Plus alloy possesses a 55
◦ C higher temperature capability in comparison to IN718 alloy. A

comparison in the chemical composition of Waspaloy alloy, IN718

alloy and 718Plus alloy is given in Table 2. Obviously, compared to
718 alloy, the main changes in chemical composition of 718Plus
alloy are the increase of Al + Ti content and Al/Ti ratio, the addi-
tion of W and Co, and the reduction of Fe element. According to
the research reported by Cao et al. [18], the volume fraction of ␥’
phase increases with the increase of Al + Ti content, while the vol-
ume fraction of ␥” phase accordingly reduced. Eventually, ␥’ phase
replaces ␥” phase as the predominant strengthening phase in 718- Fig. 6. The ␥/␥’ microstructure of a Ni3 Al-based superalloy after heat treatment.
type alloys when Al + Ti content exceeds 3 at.%. Meanwhile, the
thermal stability is improved with the increasing Al/Ti ratio. In
not revealed in Fig. 5(a) due to its extremely small size. Enlarging
the case of 718Plus alloy, the Al + Ti content is about 4 at.% and
the area which is marked as white dashed rectangle in Fig. 5(a), it
the Al/Ti ratio is approximately 4 in atomic percent, resulting in
can be observed that ␥’ precipitates exhibit a spherical morphol-
that 718Plus alloy becomes predominantly ␥’ phase strengthened.
ogy with average size of approximately 35 nm. The volume fraction
The higher temperature capability of 718Plus alloy is attributed
of ␥’ strengthening precipitates in 718Plus alloy depends on the
to the stability advantage of ␥’ phase over ␥” phase. Furthermore,
amount of grain boundary precipitates [38]. Meanwhile, the size,
the appropriate addition of Co, W, P and the reduction of Fe are
morphology, volume fraction and distribution of ␥’ precipitates are
conducive to improving stress rupture properties and thermal sta-
closely related to the variations of the heat treatment, which dis-
bility.
tinctively affects the mechanical properties of the alloy. Further
Recently, the microstructure and the relationship between
details about the evolution of ␥’ precipitate during heat treatment
microstructure and treatment of 718Plus alloy were considerably
will be discussed later.
studied [38–44]. Unlike IN718 alloy, the 718Plus alloy is predom-
inantly strengthened by ␥’ phase instead of ␥” phase. Moreover,
the main phase of grain boundary precipitates in 718Plus alloy is 3. Coarsening behavior of the ␥’ precipitate
␩(Ni3 Al0.5 Nb0.5 ) phase with a DO24 hexagonal closed pack (HCP)
crystal structure in contrast with the main grain boundary pre- In consideration of high-temperature applications, good ther-
cipitates of ı phase in IN718 alloy [45]. Fig. 5 shows the typical mal stability is required for superalloys satisfactorily serving at
microstructure of 718Plus alloy which is supplied in the form of elevated temperature. As the ␥’-strengthened alloys, the high
a forged gas turbine disc. From Fig. 5(a), the average grain size of strengths of both Ni3 Al-based alloys and 718Plus alloy are pre-
the alloy is measured as about 18 ␮m. It can be seen that many ␩ dominantly derived from ␥’ precipitates, especially for Ni3 Al-based
precipitates with plate morphology distributed not only on grain alloys with high volume fraction (above 80%) of ␥’ precipitates. The
boundaries but also in the interior of grains, as indicated by red thermal stability of these alloys rests greatly with the resistance to
arrows. In addition, few blocky precipitates proven to be M(Nb, coarsening behavior of ␥’ precipitates. Hence, it is essential to inves-
Ti)C carbides were also found precipitating on the grain bound- tigate the coarsening behavior of ␥’ precipitate in Ni3 Al-based alloy
aries, as marked by yellow arrows. The presence of ␥’ particles is and 718Plus alloy during thermal exposure.

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Y. Wu et al.
Fig. 7. The typical ␥’ + ␥ microstructures of a Ni3 Al-based alloy aged at 1000 ◦ C for various time: (a) 0.5 h; (b) 2 h; (c) 5 h; (d) 20 h.
3.1. Morphological evolution of the ’ precipitates
Over the past few decades, extensive research work about the
coarsening behavior and associated mechanisms of ␥’ precipitates
upon thermal exposure has been conducted in Ni-based alloys. As
documented on most of these previous studies, not only would the
coarsening of ␥’ precipitates occurs, but the morphology and dis-
tribution of ␥’ precipitates would evidently change as well during
the prolonged thermal exposure, leading to a further degrada-
tion of mechanical properties of alloys [46–50]. The changes in
morphology of ␥’ precipitate are attributed to the minimization
of the system’s total free energy, including the interfacial energy
and the elastic energy. To satisfy the requirement of a minimum
energy configuration, ␥’ precipitates tend to coarsen at the con-
sumption of smaller ones during the thermal exposure to reduce
the interfacial free energy, which is termed as Ostwald ripening
[51]. Additionally, the coarsened ␥’ precipitates directionally align
along the directions of lowest Young’s modulus (viz., the <100>
directions in most cubic materials) to minimize the energy asso-
ciated with the coherency straining of the lattice [52–55]. Fig. 6
presents the microstructure of a Ni3 Al-based superalloy after heat
treatment, revealing the directional alignment of cuboidal ␥’ pre-
cipitates.
In addition, it is noted that there is a close relation between
the morphology of ␥’ precipitates and its size. Small ␥’ precipi-
tates usually present spherical morphology, and the morphology
of ␥’ precipitates evolves from spherical to cuboidal or other com-
plex structures with the increasing particle size due to coarsening.
Taking the research of Ardell and Nicholson [54] as an example,
the morphology of ␥’ precipitates in Ni-6.71Al (wt.%) is converted
from spherical to cuboidal and then to plate-like with increasing
particle size during aging at 750 ◦ C and 775 ◦ C. Similar phenom-
ena were observed in many Ni-based alloys, such as the Ni-8Al
alloy by Yoem et al. [56] and Ni-Al-Cr alloy by Sudbrack et al.
[57]. However, the lattice misfit (ı) between ␥ and ␥’ phases also
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Journal of Materials Science & Technology 67 (2021) 95–104
remarkably affects the morphological evolution of ␥’ precipitates.
The ␥/␥’ lattice misfit can be calculated by the following equation:
ı= 2(a ’ − a )/(a ’ + a ), where a␥  and a␥ are the lattice parame-
ters of the ␥’ and ␥ phases, respectively. In some alloys with very
small ␥/␥’ lattice misfit, the ␥’ precipitates always remains its mor-
phology as spherical and renders independence of its particle size
[58,59]. Whereas, for some alloys with large ␥/␥’ lattice misfit, the
␥’ precipitates present a reversal coarsening characteristic that ␥’
precipitates split into smaller ones with further coarsening [60,61].
In recent years, some investigations about the coarsening
behavior of ␥’ precipitates in Ni3 Al-based alloys during thermal
aging have been conducted. Wright and Knibloe [62] reported that
the increase of annealing temperature gives rise to that the mor-
phology of ␥’ precipitates in two Ni3 Al-based alloys transfer from
blocky shape with an aspect ratio near one to regular shape. Lapin
[63] presented that the ordered ␥’-phase around the lamellas in
a directionally solidified Ni3 Al-based alloy coarsened during aging
at 1223 K, resulting in a relatively large volume fraction of lamel-
lae. Lee et al. [64] found that the ␥’ phases in an as-cast IC221 M
alloy coarsened with increasing the aging time at 900 ◦ C, and sug-
gested that coalescence was responsible for the coarsening of ␥’
phases. Li et al. [65] investigated the effect of long-term aging on
microstructure of a Ni3 Al-based single-crystal alloy IC6SX. It was
found that adjacent ␥’ phases become bigger size and connect with
each other during long-term aging at 1070 ◦ C, the ␥ phases remark-
ably coarsen as well and no longer show a continuous network-like
distribution. In our previous study [66], the coarsening behavior of
␥’ phase in the ␥’ + ␥ area of a newly developed Ni3 Al-based alloy
was explored. The typical ␥’ + ␥ microstructures of a Ni3 Al-based
alloy aged at 1000 ◦ C for various time are displayed in Fig. 7. It can
be observed that the average size of ␥’ precipitates increases with
increasing aging time when the alloy was aged at 1000 ◦ C, and cor-
respondingly, the morphology of ␥’ precipitates gradually varies
from cuboidal to strip-like and L-shaped. The width of ␥ channel
also tends to increase with the increasing aging time. In addition,
Y. Wu et al.
Fig. 8. The ␥’ + ␥ microstructures of Ni3 Al-based alloy aged at 900 ◦ C for 20 h.
the coarsening process is actually temperature dependent. Fig. 8
presents the ␥’ + ␥ microstructure of a Ni3 Al-based alloy aged at
900 ◦ C for 20 h, indicating that only a few ␥’ precipitates coa-
lesce to appear a strip-like or L-shaped morphology. By comparing
Figs. 8 and 7(d), it is evident that the coarsening of ␥’ precipitates
is accelerated by the increasing aging temperature.
In light of Allvac 718Plus alloy, Xie et al. [67] found that the main
strengthening ␥’ precipitates in 718Plus alloy present globular mor-
phology with size of in tens of nanometers. Those ␥’ precipitates
do not appreciably coarsen and the mean size of ␥’ precipitates
is still about 70 nm after thermal exposure at 760 ◦ C for 500 h,
suggesting a superior thermal stability of 718Plus alloy in compar-
ison with IN718 alloy. Whitmore et al. [42] discussed and analyzed
the effect of aging treatment on the microstructure, yield strength
and hardness of 718Plus superalloy. They found that the ␥’ pre-
cipitates grows after aging at 788 ◦ C for 4 h, and its average size
increases to 12.5 nm. As demonstrated in Fig. 9, the microstructure
of 718Plus superalloy after solution annealing and aging are shown
in dark-field model by transmission electron microscopy (TEM).
The ␥’ precipitates in both solution annealed and aged samples are
roughly spherical in morphology. Kearsey et al. [68] investigated
the microstructure of 718Plus alloy after various heat treatment
and its effects on the mechanical properties, and they reported
that the coarsening of ␥’ precipitates takes place after the ther-
mal exposure at 732 ◦ C for 1000 h. The ␥’ precipitates still keep
its morphology of near-spherical and its size not exceeds 100 nm
during coarsening. Similar experimental results have been gotten
in the investigations of Cao [38] and Löhnert et al. [69]. As men-
tioned above, the morphological transition of ␥’ precipitates from
spherical or near-spherical to cuboidal and plate-like has not be
observed in 718Plus alloy during thermal exposure. This is in large
part due to two factors: the initial particle size of ␥’ precipitates
in 718Plus alloy is much smaller than that in other Ni-based alloys
and Ni3 Al-based alloy, and good thermal stability of 718Plus alloy
at experimental temperatures.
3.2. Coarsening kinetics of the ’ precipitates
From most of previous studies on the coarsening behavior of
␥’ precipitates in Ni-based alloys [46,59,70–72], it has been com-
monly suggested that the ␥’ precipitates in Ni-based alloys coarsen
via Ostwald ripening process and the coarsening kinetics follows
classical theory developed by Lifshitz and Slyozov [73] and Wagner
[74], known collectively as the LSW theory. The classical LSW the-
ory is founded on the basis of the assumptions that: (i) the particles
are spherical with radius of R in a liquid system, (ii) the inter-
particle spacings are enormously larger than the particle radius R,
which means that there are no precipitate-precipitate interactions
between the particles and (iii) the volume fraction of the particles
is extremely low, which even approaches zero [51,73]. The LSW
100
Journal of Materials Science & Technology 67 (2021) 95–104
theory predicts a linear relationship between the cube of average
particles radius and aging time, expressed as following:
r t 3 − r0 3 = Kl ·t (1)
where t is the aging time, r0 is the initial mean particle size (t =
0) and rt is the mean particle size at time t, Kl is the coarsening
rate constant of the LSW theory. Actually, in real alloy systems,
it is impossible for particles to be zero volume fraction, and the
diffusional interactions between particles also occur, which impede
the validity of classical LSW theory.
Numerous efforts have been devoted to the modification of
LSW theory in past few decades. Taking into account the effect
of volume fraction of particles on diffusion-controlled coarsen-
ing kinetics, a modified LSW (MLSW) theory was developed by
Ardell [75]. The MLSW theory suggests that the coarsening rate
of particles increases and the theoretical distribution of particle
sizes tends to be broader as its volume faction increases. In fact,
the MLSW theory inflates the effect of volume fraction on the
growth rate constant, which is inconsistent with the experimen-
tal results. Furthermore, the adjacent ␥’ particles may approach
and even encounter each other when the ␥’ particles coarsen incre-
mentally during prolonged thermal exposure. Hence, based on the
assumption of instantaneous coalescence of precipitates, Davies
et al. modified the classical LSW theory and proposed the Lifshitz-
Slyozov encounter modified (LSEM) model [76]. According to the
LSEM model, the coarsening rate of particles increases to a small
extent and the particle-size distribution also becomes broader due
to the coalescence of particles. Moreover, the cube of average par-
ticle radius still increases linearly with the aging time in LSEM
model, just like the classical LSW model. Recently, a new vol-
ume fraction independent coarsening model was introduced by
Ardell and Ozolins [77], named Trans-Interface Diffusion Controlled
(TIDC) coarsening model, involving solute diffusion through the
disordered–ordered ␥/␥’ interface rather than through the disor-
dered ␥ matrix. It is suggested that diffusion of solute atoms in
partially ordered ␥/␥’ interfaces is much slower than in disordered
␥ matrix. Differing from those previous coarsening models, the
TIDC model indicates that the square of average particle radius is
proportional to the aging time, which is written as following:
rt 2 − r0 2 = Ki ·t (2)
where Ki is the coarsening rate coefficient of TIDC model, and all
the other parameters in Eq. (2) have the same meaning as in Eq.
(1). More recently, the coarsening of ␥’ precipitates in some Ni-
based alloys was examined to be coincided with the TIDC model
[50,78,79]. All the coarsening models, mentioned above, suggest
that the change in average particle radius follows a temporal power
law during coarsening process, i.e. (rt n − r0 n )∝t, where n is the
temporal exponent. The various values of n are corresponded with
different coarsening mechanism: the value of n is expected to be
3 for the matrix-diffusion-controlled coarsening (as LSW, MLSW
and LSEM model) and 2 for the trans-interface-diffusion-controlled
(TIDC) coarsening.
In spite of the fact that the elastic energy exists during the coars-
ening process and the volume fraction of ␥’ precipitates is relatively
high, many previous literatures have demonstrated that the coars-
ening kinetic of ␥’ precipitates in Ni3 Al-based alloys and 718Plus
alloy are nevertheless in accordance with the temporal laws of the
classical LSW theory. Motejadded et al. [80] investigated the coars-
ening kinetics of ␥’ precipitates in dendrite regions of IC221 M alloy.
It was reported that the coarsening process of ␥’ precipitates in
IC221 M alloy follows the LSW theory and the calculated activation
energy of 253.5 kJ/mol indicated that ␥’ precipitates coarsening
is controlled by volume diffusion of Al (the diffusion activation
energy of Al in Ni-matrix is 284 kJ/mol). Ai et al. [81] studied the
effect of heat treatment on the microstructure of a Re-containing
Y. Wu et al.
Fig. 9. The TEM dark-field micrographs of 718Plus superalloy after (a) solution annealing at 980 ◦ C for 30 min and (b) aging at 788 ◦ C for 4 h, adapted from Ref. [42].
Fig. 10. The scatter plot of the lnr vs. lnt for a Ni3 Al-based alloy under various aging
conditions.
Ni3 Al-based single crystal alloy. Moreover, a comparative study of
the LSW and TIDC models was performed. The results indicated
that the LSW model is superior to TIDC model in describing the
coarsening behavior of ␥’ precipitates, implying the ␥’ precipitates
coarsening is predominantly controlled by the volume diffusion
instead of the trans-interface diffusion. Our research group have
also researched the coarsening kinetics of ␥’ precipitates in the ␥’ +
␥ area of a Ni3 Al-based alloy [66]. Unlike findings from other pre-
vious studies on the similar subject, we found that the process of
␥’ precipitates coarsening can be divided into two stages, including
early stage and later stage. This is inferred from the fact that the
turning points are viewed on various aging temperatures of the ln
r vs. ln t scatter plots, as illustrated in Fig. 10. From Fig. 10, it can
also be found that the turning point occurs earlier with the increas-
ing temperature. Based on the experimental data, LSEM model and
TIDC model were applied to predict the kinetics of two coarsening
stages. The fitting results presented that the cube rate law of LSEM
model fits better for the early stage coarsening, while the square
rate law of TIDC model fits better for the later stage coarsening. In
addition, the activation energies were evaluated as 174.2 kJ/mol
and 186.3 kJ/mol for the early stage and later stage coarsening,
respectively.
With regard to the coarsening kinetics of ␥’ precipitates, only
a few studies have hitherto been conducted on the 718Plus alloy.
The microstructural characterization of ␥’ precipitates in 718Plus
alloy after aging treatment at various temperature (from 1048 K to
1223 K) was investigated by Zickler et al. [82]. The results revealed
that the particle radius ␥’ precipitates coarsens as the aging time
101
Journal of Materials Science & Technology 67 (2021) 95–104
increases, and there is a linear relationship between the particle
radius and the cube root of aging time. Besides, a modified LSW
theory introduced by Calderon et al. [83] was applied to deter-
mine the activation energy for ␥’ precipitates coarsening as 303
kJ/mol. Löhnert et al. [69] have also stated that the coarsening of
␥’ precipitates in 718Plus alloy follows the LSW type relationship,
i.e. the particle radius increases proportionally to the cube root of
aging time. Besides, Wang et al. [84] performed a computational
kinetics simulation of the precipitation and dissolution of ␥’ pre-
cipitates in 718Plus alloy during aging and welding. It was testified
that the calculated particle radius increases with the increase of
aging time, and the calculated results was found to be consistent
with the experimental results reported by Zickler et al. [82].
4. Hot deformation behavior of ␥’-strengthened
superalloys
In the following, the deformation behavior of the ␥’-
strengthened Ni3 Al-based and 718Plus superalloys will be
discussed, and the variation in deformation behavior and the cor-
responding changes of deformed microstructure derived from the
␥’ precipitates coarsening will be studied.
4.1. Hot deformation behavior
In general, the deformation parameters (i.e. deformation tem-
perature, strain rate and strain) have a significant influence on the
properties of alloys. Thus, the deformation parameters should be
stringently controlled during the thermomechanical processing of
alloys to achieve superior performance. Over past few decades, a
great number of researches about the hot deformation behavior
have been carried out on some Ni-based alloys [11,85–87]. But as
the newly developed superalloys, there are limited investigations
focusing on the thermal deformation behavior and workability of
the Ni3 Al-based alloys and Ni-based 718Plus alloy.
Sikka et al. [88] have studied the hot forging processing of alloy
IC218LZr, and they found that the unexposed alloy performed bet-
ter workability during hot forging than the alloy exposed to 1200 ◦ C.
Based on the dynamic materials model (DMM), the processing maps
have been confirmed to be an effective tool for optimizing the pro-
cessing parameters and predicting the “safe” working domain and
“unsafe” working domain during hot-working processes of met-
als and alloys [89–92]. Prasad et al. [93] have characterized the
hot deformation behavior of the as-cast IC396LZr alloy. The char-
acteristics of the flow curves, kinetic analysis and processing maps
were studied. The results revealed that the DRX occurs at the con-
dition of 1250 ◦ C/0.001 s−1 which is considered to be desirable
Y. Wu et al. Journal of Materials Science & Technology 67 (2021) 95–104

Fig. 11. (a) The processing map of a Ni3 Al-based alloy at a strain of 0.8 and (b-f) the deformed microstructures which correspond to the different domains indicated by red
arrows in the processing map, adapted from Ref. [29].

Fig. 12. TEM micrographs of the Ni3 Al-based alloy with different initial microstructure: (a) fine cuboidal ␥ precipitates; (b) coarse strip-like ␥ precipitates.

for hot working of this alloy. Besides, in the investigation of Wang
et al. [94], the flow curves of Ni3 Al-based alloy MX246A during hot
compression tests have been analyzed and the processing maps
have also been established. According to the processing map of the
true strain of 0.7, the safe domain for hot working was determined
as the deformation temperature of about 1220 ◦ C with the strain
rate of 0.001 s−1 . Recently, in our previous investigation [29], the
hot deformation behavior of a newly developed Ni3 Al-based alloy
have been explored. Almost all the flow curves showed the typi-
cal DRX characteristics that the flow stress reaches a peak value at
the critical strain and followed by an obvious flow softening with
further straining. To elucidate the relationship between the flow
stress, strain rate and deformation temperature at a given strain,
a constitutive equation was also calculated by using a hyperbolic-
sine type Arrhenius equation. Moreover, the processing maps of
the studied alloy were obtained and the corresponding deformed
microstructures for different domains in the processing map were
characterized, as displayed in Fig. 11, in which the gray areas signify
the instability domains. It can be seen that there are two insta-
bility domains in the processing map, which are symbolized as A
and B in Fig. 11, respectively. Further microstructure observation
of these instability domains revealed the presence of instability
phenomena, such as flow localization, adiabatic shear bands and
cracks. Generally, the area with higher power dissipation factor
(␩, represented by the contour numbers in processing maps) value
corresponds to the better processing performance area. It can be
clearly observed from Fig. 11 that there is a high ␩ region in the
range of deformation temperature of 1250 ◦ C and strain rate range
of 0.01−0.1 s−1 . Combined with the microstructure observation, it
is found that the deformed microstructure under this deformation
condition is a fully recrystallized structure, and the recrystallized
grains are fine and uniform. Therefore, it can be determined that the
processing parameters corresponding to this region are the opti-
mized parameters for the hot working processing of Ni3 Al-based
alloy.
Regarding to the deformation behavior of the 718Plus superal-
loy, Huber et al. [95] have performed hot compression tests at a
temperature range of 900–1050 ◦ C with the strain rates of 0.1–10
s−1 and characterized the hot deformation behavior of 718Plus
alloy. The flow curve modeling was studied and the deformation
activation energy was determined as 430.0 kJ/mol. Besides, by opti-
cal microscopy observation and EBSD analysis, it was revealed the
increase of DRX fraction with increasing strain. Ozturk et al. [96]
have investigated the precipitation and flow behavior of 718Plus
alloy during hot compression tests. The flow curves revealed that
the critical stress for DRX initiation decreases with the increas-
ing deformation temperature. The activation energy of deformation
was calculated as 525.5 kJ/mol by using hyperbolic sine model. And

102
Y. Wu et al.
Fig. 13. The flow curves and deformed microstructures of the studied alloys with
different initial microstructures deformed at various conditions, in which dot lines
and solid lines represent the studied alloy with fine cuboidal ␥ precipitates and
coarse strip-like ␥ precipitates, respectively.
it was concluded that the deformation process of 718Plus alloy is
controlled by self-diffusion of Ni atoms.
4.2. Effects of the ’ precipitates coarsening on hot deformation
behavior
The Ni3 Al-based alloys and Ni-based 718Plus alloy are primarily
strengthened by the ␥’ precipitates. As mentioned above, the coars-
ening of ␥’ precipitates usually occurs during the thermal exposure,
resulting in the changes in size, morphology and precipitate size
distribution (PSD) of ␥’ precipitates, which can significantly affect
the mechanical properties of alloys. Therefore, investigations on
variations of the deformation behavior from ␥’ precipitates coars-
ening possess significances for adjusting process parameters and
improving the performance of these ␥’-strengthened superalloys.
Sun et al. [97] observed the coarsening of ␥’ precipitates in
Ni-based U720Li superalloy heated at 1130 ◦ C, and demonstrated
that there were distinct changes in size, morphology and volume
fraction of ␥’ precipitates due to coarsening process, which sig-
nificantly affects the hot deformation resistance of the alloy. As
the deformation temperature increased to above 1150 ◦ C, the flow
stress was decreased with the increasing deformation tempera-
ture, which could be attributed to the dissolution of ␥’ precipitates.
Zhang et al. [98] stated that the dense fine ␥’ precipitates which
formed in the solution treated powder metallurgy Ni-based super-
alloy FGH96 resulted in higher deformation resistance. With the
increasing deformation temperatures, the difference between the
flow stresses of hot isostatic pressed and solution treated samples
reduced due to the dissolution of ␥’ precipitates. In our previous
work [99], the comparative study of hot deformation characteristics
and corresponding microstructure evolution for the Ni3 Al-based
alloy with different initial microstructures (i.e. different size and
morphology of ␥’ precipitates) was conducted. It is concluded that
the initial microstructure can significantly affects the hot defor-
mation behavior of the Ni3 Al-based alloy. The different initial
microstructures of the studied alloys are exhibited in Fig. 12, show-
ing fine cuboidal ␥ precipitates and coarse strip-like ␥ precipitates.
Fig. 13 demonstrates the flow curves of the Ni3 Al-based alloy with
different initial microstructure deformed at various conditions. It
can be clearly observed that both the peak stress and the mag-
nitude of the stress drop for the alloy with coarse strip-like ␥
precipitates are higher than those for the alloy with fine cuboidal
␥ precipitates at a constant deformation temperature and strain
rate. This result indicates the coarse ␥ precipitates improved the
degree of dynamic recrystallization (DRX) process, which is further
substantiated by microstructure observation, as depicted in Fig. 13.
103
Journal of Materials Science & Technology 67 (2021) 95–104
Besides, in accordance with the results of Sun et al. [97] and Zhang
et al. [98], the flow curves present the weaken effect of different ␥
precipitates on hot deformation behavior under the deformation
condition of 1200 ◦ C/1 s−1 , which could be due to the dissolution of
coarse ␥ precipitates at the higher temperature. The critical con-
dition for the initiation of DRX in the studied alloy with different
initial microstructure was also confirmed and a summing-up for the
effect of initial microstructure on the critical condition of DRX was
given. It is found that the alloy with coarse ␥ precipitates presents
higher critical stress and strain value. This is ascribed to that the
dislocation movement can be inhibited by the coarse strip-like ␥
precipitates during hot deformation.
5. Concluding remarks
The ␥ -strengthened superalloys possess excellent mechanical
properties as well as good corrosion resistance at elevated temper-
ature, which makes it ideal for high temperature applications. It is
widely accepted that these alloys derive high strength from the ␥
precipitates with ordered L12 crystal structure. Hence, the evolu-
tion in morphology, size and distribution of ␥ precipitates during
the coarsening process can significantly affect the properties of ␥ -
strengthened superalloys. For these considerations, an overview on
the coarsening of ␥ precipitates and its effects on the hot deforma-
tion behavior of two newly developed ␥ -strengthened superalloys,
i.e. Ni3 Al-based intermetallic alloys and Allvac 718Plus superalloy,
has been presented in this paper.
During thermal exposure, the occurrence of ␥ precipitates
coarsening can be found in Ni3 Al-based alloys and 718Plus super-
alloy. The morphology of ␥’ precipitates during coarsening is
collectively controlled by the interfacial energy and the elastic
energy, and it is closely related to the particle size and the ␥/␥’
lattice misfit. During coarsening, the morphology of ␥’ precipitates
evolves from cuboidal to strip-like or other complex structures in
Ni3 Al-based alloys, while the ␥’ precipitates in 718Plus alloy always
present near-spherical morphology due to the relatively small par-
ticle size. Meanwhile, the temporal evolution of average size of the
␥’ precipitates in 718Plus alloy follows the classical LSW theory.
In Ni3 Al-based alloys, the coarsening mechanism of ␥’ precipi-
tates is affected by the increasing ␥’ size and widened ␥ channel
due to coarsening. The coarsening process of Ni3 Al-based alloy is
divided into two stages, i.e. early stage and later stage, following
the cube rate law of LSW theory and the square rate law of TIDC
theory, respectively. Furthermore, the hot deformation behavior
of Ni3 Al-based alloys and 718Plus superalloy are reviewed, and
the variations of hot deformation behavior of alloys derived from
hot deformation behavior coarsening are discussed. It is concluded
that the hot deformation behavior of ␥ -strengthened superalloy is
greatly influenced by the coarsening of ␥ precipitates.
In summary, this review may provide some practical sugges-
tions for microstructure design and properties optimization of
␥ -strengthened alloys. In this article, we have mostly discussed
the ␥ precipitates coarsening and its effects on the hot deformation
behavior of these alloys. Considering the increasing computational
power, simulations about the defect evolution and phase trans-
formation should be paid attention to. To further improve the
mechanical performances and promote more extensive applica-
tions of these ␥ -strengthened superalloys, more experimental and
computational studies concerning the ␥’ precipitates coarsening
kinetics and the underlying coarsening mechanism, as well as its
effect on other properties, such as strength, creep resistance and
tensile etc. are required in the future. Besides, the mechanical prop-
erties of these alloys are sensitive to the volume fraction and size
of ordered ␥ precipitates, which calls for further investigations
regarding microstructure optimization by the addition of alloying
Y. Wu et al.
elements or heat treatment. As for the ␥ -strengthened intermetal-
lic superalloys, such as Ni3 Al and Co3 Al, their applications are still
restricted to a great extent due to its intrinsic brittleness at or
below room temperature. Therefore, fundamental studies on the
strengthening and toughening of these intermetallic alloys also
should be performed in future works.
Acknowledgements
This work was supported financially by the National Natural Sci-
ence Foundation of China (Nos. 51474156 and U1660201) and the
National High Technology Research and Development Program of
China (No. 2015AA042504).
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