Journal of Alloys and Compounds 930 (2023) 167522

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Journal of Alloys and Compounds

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Influence of heat treatment on Inconel 625 superalloy sheet: carbides, γ'',

δ phase precipitation and tensile deformation behavior ]]
]]]]]]
]]

⁎
Xudong Liu a, Jiangkun Fan a,b,c, , Peizhe Zhang a, Kai Cao a, Zixiao Wang a, Fulong Chen a,d
⁎
Degui Liu d, Bin Tang a,b,c, Hongchao Kou a,b,c, Jinshan Li a,b,c,
a
State Key Laboratory of Solidification Processing, Northwestern Polytechnical University, Xi’an 710072, PR China
b
National & Local Joint Engineering Research Center for Precision Thermoforming Technology of Advanced Metal Materials, Xi’an 710072, PR China
c
Innovation Center, NPU·Chongqing, Chongqing 401135, PR China
d
AVIC Manufacturing Technology Institute, Beijing 100024, PR China

a r t i cl e i nfo a bstr ac t

Article history: In this study, commercial Inconel 625 superalloy was subjected to solution and longer-term aged treatment.
Received 13 July 2022 The effects of the temperature and time of aged treatment on the secondary-phase evolutions, tensile
Received in revised form 1 September 2022 properties, and strengthening mechanism of Inconel 625 superalloy were systematically investigated. The
Accepted 7 October 2022
results showed that the evolution of M23C6 carbides mainly included two paths: MC+ γ→M23C6 at 650 °C
Available online 10 October 2022
and MC+ γ→M23C6 + δ at 750 °C. The disk-like γ'' phase with three mutually orthogonal variants dispersedly
precipitated within the grains after aged treatment at 650 °C for 200 h. After aged treatment at 750 °C for
Keywords:
Inconel 625 100 h, the needle-like δ phase parallelly precipitated around the grain boundaries. As the aged time reached
Carbides 200 h and 300 h, δ phases precipitated within the grains at the expense of the metastable γ" phase. Both γ''
γ'' phase and δ phases strengthened the alloy during tensile deformation at room temperature (RT). However, the γ''
δ phase phase showed a better strengthening effect than the δ phase. Coarsened δ phases would cause severe stress
Strengthening mechanism concentration around δ phase/matrix interfaces during the non-uniform deformation stage. With the in­
crease of tensile strain, many microvoids appeared around the δ phases/matrix interfaces, which weakened
the strengthening effects of the δ phases.
© 2022 Elsevier B.V. All rights reserved.

1. Introduction rich in Nb and Mo) and M23C6 (“M” is rich in Cr) carbides are
transformed from the MC carbide during aged treatment [7–9]. The
Inconel 625 alloy is a solid-solution strengthened nickel-based main strengthening phase of Inconel 625 alloy is the coherent and
superalloy, widely used in the petrochemical, aerospace, marine, ordered metastable γ″ (Ni3Nb) phase with a body-centered tetra­
power generation, and nuclear industries due to its excellent high- gonal D022 structure [10]. δ (Ni3Nb) phase with a D0a orthorhombic
temperature strength and corrosion resistance [1–4]. Cr, Mo, Fe, and structure is the equilibrium phase of γ″ and is more stable than the
Nb are the representatives of the solid solution strengthening ele­ γ″ phase [11].
ments in Inconel 625 alloy. Cr and Mo can improve the corrosion The precipitation phases such as carbide, γ″, and δ phases are
resistance of the alloy, Fe reduces cost, and Nb facilitates precipita­ important for the mechanical properties of Inconel 625 alloy due to
tion hardening [5,6]. Inconel 625 alloy usually serves at elevated the complicated evolution of precipitation phases during thermal
temperatures, and its microstructure is highly likely to change in a aged. Therefore, the in-depth revelation of secondary-phase pre­
complex environment. Previous studies show five typical pre­ cipitation and its impact on mechanical properties are extremely
cipitates (primary MC carbide, secondary M6C, M23C6 carbides, γ'', important for the processing and application of Inconel 625 alloy.
and δ phases) in the γ matrix [2,4]. The chemical composition of The effect of temperature and time on the evolution of precipitation
these precipitates is summarized as follows. MC (“M” is rich in Nb) phases in Ni-based superalloys with the consideration of the re­
carbide is generated during solidification. Secondary M6C (“M” is lationship between precipitation phases and mechanical properties
has been investigated in many studies.
Suave et al. [12] found that the precipitation temperature of the
⁎
Corresponding authors at: State Key Laboratory of Solidification Processing, γ″ phase was between 550 °C and 750 °C, and the growth of the γ″
Northwestern Polytechnical University, Xi’an 710072, PR China. phase followed the Lifshitz theory once its morphology altered from
E-mail addresses: [email protected] (J. Fan), [email protected] (J. Li).

https://doi.org/10.1016/j.jallcom.2022.167522
0925-8388/© 2022 Elsevier B.V. All rights reserved.
X. Liu, J. Fan, P. Zhang et al. Journal of Alloys and Compounds 930 (2023) 167522

Table 1
Chemical compositions of the Inconel 625 superalloy (wt%).

Ni Cr Mo Nb Fe Al Si C Ta Ti Mn

60.74 21.71 8.93 3.32 4.22 0.52 0.41 0.040 < 0.01 0.21 0.41

spheroidal shape to lens-like shape. In addition, the γ'' phase would Table 2
connect and transform into the δ phase after aged treatment at Aged treatment parameters performed on Inconel 625 alloy.
650 °C for 2000 h. He et al. [13] observed three variants of the γ″ 25 h 50 h 100 h 200 h 300 h 400 h
phase in Ni-Co-Cr-Fe-Nb alloy after aged at 650 °C for 80 h. Com­ 650 °C √ √ √
pared with solution-treated alloy, the yield strength (YS) and ulti­ 750 °C √ √ √ √ √
mate tensile strength (UTS) of the aged alloy were increased by
670 MPa and 520 MPa, respectively. Zhang et al. [14] tailored the
variant and shape of the γ″ phase by cold rolling and aged treatment 2. Experimental material and procedure
in Inconel 718 alloy. Creep tests have proved that an orientation-
specific γ″ variant substantially can improve creep resistance at A rolled Inconel 625 sheet with a thickness of 5 mm was adopted
650 °C, which is superior to the creep resistance improved by in this study. Its chemical composition is shown in Table 1. Before
commonly perpendicular γ″ variants. δ phase will transform from aged treatments, specimens were heated to the solution tempera­
the γ″ phase at a relatively low temperature or precipitate directly ture (1100 °C) and held for 60 min, and then these specimens were
from the γ matrix at a higher temperature [15–17]. Rao et al. [18] water-quenched to room temperature (RT). The specimens were
found that the coarse δ phase could degrade the strength of Inconel aged at 650 °C and 750 °C for time durations from 25 to 400 h. The
718 alloy due to the corresponding depletion of the γ″ phase. Lin results are shown in Table 2.
et al. [19] studied the relationship between the δ phase and dynamic Tensile specimens measuring 2 mm × 30 mm × 5 mm (thickness
recrystallization (DRX) grains in the GH4169 alloy. The result showed × gauge length × width) were processed by electrical discharge
that δ phases could easily induce high-density dislocation cells, thus machining according to GB/T 228.2–2015 standard. Tensile tests
accelerating the formation of DRX grains. Saarimäki et al. [20] found were performed at RT using an Instron 5982 universal testing ma­
that the growth rates of fatigue crack were strongly dependent on δ chine, giving a nominal strain rate of 1.2 × 10−3 s−1. Engineering
phase orientation. When δ phases are perpendicular to the loading stress-strain curves were drawn using the original data. The areas
direction, the crack growth rates are approximately ten times faster 5 mm away from the fractured surface of the specimens were se­
than that parallel to the loading direction. Ning et al. [21] reported lected for microstructural characterization.
that the shape of the δ phase could greatly affect the mechanical The scanning electron microscope (SEM: ZEISS Gemini 500)
property of Inconel 718 superalloy. Stick δ phases show good plas­ equipped with an electron backscattered diffraction (EBSD) camera
ticity while the needle δ phase owns high strength. (Oxford Instruments) and an energy dispersive X-ray spectrometer
Motivated by the recent reports, the mechanical properties of Ni- (EDS) was used for analyzing microstructure morphologies, grain
based superalloys are strongly dependent on the type, size, and orientations, and elemental compositions. A conventional metallo­
crystal orientation of secondary-phases. The coherent and ordered graphic preparation technique was adopted to prepare the SEM and
metastable γ″ phase can strengthen the alloy, but it is a metastable EDS specimens. For the EBSD tests, the mirror-polished samples
phase and is easily transformed into the δ phase. The precipitation of were further polished using a vibratory polisher (Buehler, VibroMet
δ phase at grain boundary sometimes is believed to resist crack 2) for 5 h to remove surface stress. The EBSD orientation data were
propagation and thusly improve the rupture stress. On the other acquired at an accelerating voltage of 20 kV and a step size of 0.4 µm.
hand, with the increasing of size, coarse and incoherent δ phase are Channel 5.0 software was used to analyze the EBSD measurements.
easy to become crack nucleation sites in latter half of the deforma­ Thin foil specimens with a thickness of 60 µm for transmission
tion, which deteriorates UTS and elongation. Up to now, the past electron microscopy (TEM) investigations were prepared by hand
works have provided excellent investigations about the secondary- grinding. Further thinning was achieved through a twin jet polishing
phase evolution in some nickel-based superalloys. Nevertheless, the technique with a solution of 10% perchloric acid + 90% alcohol at
relationship between γ″→ δ phase transformation characteristics and − 30 °C and 25 V. The TEM observations were performed using an FEI
temperature/time have been still rather limited, particularly the Talos F200X microscope operating at 200 kV.
crystallographic features, size and volume fraction of γ″ and δ
phases. In addition, since both γ″ and δ phases can strengthen the
alloy to some extent, an issue of which one shows better strength­ 3. Results and discussions
ening effect is still unclear. Furthermore, unlike Inconel 718 and
other nickel-based alloys, the content of Cr (∼23 wt%) and Mo (∼9 wt 3.1. Solution treatment
%) in Inconel 625 is high, which makes the precipitation behavior of
carbides very complex. Considering the issues mentioned above, the Fig. 1(a) and 2 show the typical microstructures of the initial
characteristics of secondary-phase precipitation and the relationship Inconel 625 alloy. As shown in Fig. 1(a), the microstructure of the
between secondary-phase and tensile properties should be further initial Inconel 625 alloy consists of a few coarse deformation grains,
studied to provide reliable data support for the selection of heat fine recrystallized grains, and annealing twins. As shown in Fig. 2(a)
treatment parameters of Inconel 625 alloy. and 2(b), some block (Point 1) and granular (Point 2) precipitate
In this work, different kinds of secondary-phases, including car­ irregularity distribute around grain boundaries. According to the
bides, γ″, and δ phases, were obtained through the solution and aged results of EDS analysis, granular precipitates with a size of < 1 µm
treatment at different temperatures. The effect of aged temperature and block precipitates with a large size were classified as Nb-rich
and time on secondary-phase evolution was deeply investigated. In carbides [22]. The atomic percent obtained by EDS characterizations
addition, the effect of γ″ and δ phases on tensile properties and is shown in Table 3. In addition, the EDS analysis of the matrix (Point
corresponding strengthening mechanisms was systematically re­ 3) is almost consistent with the nominal composition of Inconel 625
searched. superalloy. According to Fig. 1(a), the initial average grain size of

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X. Liu, J. Fan, P. Zhang et al. Journal of Alloys and Compounds 930 (2023) 167522

Table 3
Atomic percent (at%) obtained by EDS characterizations in Fig. 2.

Point Ni C Nb Ti Cr Mo Fe

1 1.5 50.8 44.3 2.3 1.1 0 0

2 6.6 42.1 45.6 3.6 2.1 0 0
3 61.5 0 2.5 0.2 22.3 8.9 4.6

the type of secondary carbides. The types of carbides can be de­

termined by elemental analysis. M23C6 and M6C carbide are rich in
Cr and Mo, respectively [23,24]. The chain secondary carbides at
grain boundaries were divided into two parts: rich Cr areas (M23C6
carbides) and rich Mo areas (M6C carbides) (Fig. 3(e)− 3(g)). The
result can also be proved by the corresponding SAED patterns in
Fig. 3(h) and 3(i). Fig. 4 presents the secondary carbides at grain
boundaries of specimens aged at 650 °C for 300 h. Secondary car­
bides were classified as M23C6 and M6C carbides by elemental and
SAED patterns analysis. Therefore, the carbides at the grain
boundary were M23C6 and M6C carbides after aged at 650 °C
and 750 °C.

Fig. 1. IPF maps of various microstructure after solution treatments at 1100 °C: (a) 3.3. Transformation of primary MC carbide
initial specimen; (b) 10 min; (c) 60 min; (d) 120 min.
The thermal stability of primary MC carbide decreases at high
Inconel 625 alloy can be calculated as 25 µm without considering temperatures. M23C6 carbides and δ phase can be transformed from
twin boundaries. the primary MC carbide after aged treatment. There are two dif­
In order to obtain the supersaturated solid solution, the initial ferent evolution paths of MC carbide: MC+ γ→M23C6 and MC+ γ→
sheet was subjected to solution treatment. Fig. 1(b)-(d) illustrate M23C6 + δ at different temperatures.
inverse pole figure (IPF) maps of the specimen treated at 1100 °C for
various time. Fig. 1(b) indicates that the coarse deformation grains 3.3.1. First path of MC carbide evolution: MC+ γ→M23C6
are gradually replaced by many fine austenite equiaxed grains after Fig. 5 presents the evolution of primary MC carbide in the Inconel
10 min solution treatment. As shown in Fig. 1(c), the average grain 625 alloy aged at 650 °C for 300 h. The yellow area in Fig. 5(a) and
size does not significantly increase after solution treatment at 5(b) shows that some black particles are formed inside the bright
1100 °C for 60 min. As the solution treatment time increases from bulk-shaped carbide. According to the corresponding EDS composi­
60 min to 120 min, the grains grow rapidly during the subsequent tional maps (Fig. 5(c)− 5(e)) and SAED analyses (Fig. 5(f)), the black
solution, and the average grain size significantly increases from particles and the bright bulk-shaped carbide represent Cr-rich M23C6
20 µm to 45 µm, as shown in Fig. 1(d). Therefore, 1100 °C/60 min was and NbC, respectively. The SAED pattern shows that M23C6 and MC
selected as an appropriate treatment parameter to obtain super­ carbides with FCC crystal structure present a cube-on-cube or­
saturated solid solution and fine grains. ientation relationship [25], i.e [112]M23C6//[112]MC and (111) MC //
(333) M23C6. Therefore, the microstructure evolution of the primary
3.2. Secondary carbides at grain boundaries MC carbide can be summarized as MC+ γ→M23C6 in Inconel 625 alloy
aged at 650 °C.
The SEM and TEM observation for the specimens after aged
treatment at 750 °C from 25 h to 300 h is illustrated in Fig. 3. As 3.3.2. Second path of MC carbide evolution: MC+ γ→M23C6 + δ
shown in Fig. 3(a), a small number of secondary carbides precipitate Fig. 6 reveals the microstructure evolution of the primary MC
at the grain boundaries after 25 h aged treatment at 750 °C. In carbide aged at 750 °C for 100 h. The yellow box area shows that Cr-
Fig. 3(b), the secondary carbides grow rapidly into blocks and con­ rich M23C6 carbides precipitate inside NbC, while the needle-like δ
nect into chain carbides between 25 and 100 h. The growth rate of (Ni3Nb) phase nucleates and grows on the edge of MC carbide ac­
secondary carbides declines significantly after 100 h, as shown in cording to the SEM micrograph (Fig. 6(a)) and EDS mappings
Fig. 3(c). Fig. 3(d) shows the High-Angle Annular Dark Field (HAADF) (Fig. 6(b) and 6(c)). The result indicates the path of microstructure
image of blocky carbides around grain boundaries after aged treat­ evolution: MC+ γ→M23C6 + δ at 750 °C. Fig. 6(d)− 6(f) further confirm
ment at 750 °C for 50 h. The EDS maps and selected area electron that the Nb-rich needle-like δ phase is transformed from MC carbide
diffraction (SAED) patterns are illustrated in Fig. 3(e)− 3(i) to reveal by EDS maps (Fig. 6(e)) and the SAED pattern (Fig. 6(f)).

Fig. 2. Initial microstructure of the studied Inconel 625 sheet. (a) SEM image; (b) BSE image of NbC and corresponding EDS elemental maps.

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X. Liu, J. Fan, P. Zhang et al. Journal of Alloys and Compounds 930 (2023) 167522

Fig. 3. SEM micrograph of the secondary carbides nucleation and growth after aged treatments at 750 °C: (a) 25 h; (b) 100 h; (c) 300 h; (d) HAADF image of secondary carbides
after aged treatments at 750 °C for 50 h; corresponding EDS elemental maps for Fig. 3(d) showing the distributions of (e) Cr / Mo, (f) Cr, and (g) Mo; (h) [011]M23C6 orientated SAED
pattern of area 1 in Fig. 3(f); (i) [011]γ orientated SAED pattern of area 2 in Fig. 3(g).

Fig. 4. Bright-field images, EDS elemental mapping and corresponding SAED patterns after aged treatment at 650 °C for 300 h: (a) Bright-field image; (b) HAADF image; (c, d) EDS
maps of the area indicated in the yellow box in (b); (e) the SAED pattern of area 1 in (d); (f) the SAED pattern of area 2 in (d).

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X. Liu, J. Fan, P. Zhang et al. Journal of Alloys and Compounds 930 (2023) 167522

Primary MC carbide evolution modes at different temperatures

are illustrated in Fig. 7. The classical reaction: MC+ γ→M23C6 + γ' and
MC+ γ→M6C+ γ' were found in various superalloys [26,27]. Al and Ti
usually promote the formation of γ′ phase in Ni-based alloy. For the
studied Inconel 625 alloy, the low content of Al (∼ 0.53 wt%) and Ti
(∼ 0.21 wt%) makes the γ' phases difficult to be observed, which is
consistent with the results reported by Yu et. al [28]. The thermal
stability of primary MC carbide decreases significantly with the in­
crease of thermal exposure temperature [29]. The primary MC car­
bides degeneration is an element diffusion-controlled process. The
main alloying element of MC carbides is Nb, which diffuses to the
matrix. Meanwhile, the Cr element in the matrix diffuses into the MC
carbide to increase the ratio of Cr/Nb in MC carbides. The MC car­
bides react with the matrix to form M23C6 carbides under 650 °C and
750 °C aged treatment: MC+ γ→M23C6.
Furthermore, the δ phase nucleates and grows at the interface
between MC carbide and matrix due to the enrichment of Nb ele­
ments after aged at 750 °C. The δ phase is transformed from the γ''
phase under 800 °C aged treatment in Inconel 625 alloy [30]. The
thermodynamic energy provided by temperature is insufficient to
overcome the energy barrier for the δ phase direct precipitation
from the matrix under 750 °C. Therefore, the metastable γ'' phase
must be precipitated before the phase transition progress: γ''→δ [31].
δ phase can be directly transformed from MC carbide during aged
treatment because the high lattice distortion energy between the
MC carbide/matrix interface provides enough energy fluctuations.
Similarly, the η phase precipitates on the phase boundary between
MC and γ' and grows at the expense of both γ' and MC in a Waspaloy
Ni-based superalloy [32].

3.4. γ'' phase precipitation

Fig. 8(a) shows the nucleation of disk-like γ'' (Ni3Nb) phase par­
ticles within the grains after aged at 650 °C for 200 h. The γ'' phase
shows a D022 lattice, which is composed of two FCC unit cells placed
Fig. 5. Evolution of primary carbide at 650 °C for 300 h. Comprehensive character­
one over another along the [001] direction. The eight corners and the
ization of the M23C6 carbide formation in MC carbide using TEM: (a) Bright-field
image; (b) HAADF image of a magnified area marked as a yellow box in (a); EDS center of the body-centered tetragonal (BCT) unit cell are placed by
elemental maps for Fig. 5(b) showing the distributions of (c) Nb, (d) Cr, and (e) Cr/Nb; Ni atoms, while the rest sites are occupied by Nb atoms [33]. The
(f) SAED pattern of the area marked as a red circle in Fig. 5(e). SAED maps of γ'' phase variants are shown in Fig. 8(b). The

Fig. 6. Evolution of primary carbides after aged at 750 °C for 100 h. Comprehensive characterization of the M23C6 carbide and δ phase formation in MC carbide using SEM and
TEM: (a) SEM micrograph of δ phases and carbides; (b, c) EDS mapping of Cr and Nb, (d) HADDF image of δ phases and NbC; (e) Nb element distribution map; (f) the SAED pattern
of δ phase.

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X. Liu, J. Fan, P. Zhang et al. Journal of Alloys and Compounds 930 (2023) 167522

Fig. 7. Schematic illustrations of the evolution modes of MC carbide at different temperatures.

crystallographic relations between the γ'' phase and matrix are as

follows: spot 1 represents the [001]γ//[010]γ'', spot 2 represents the
[001]γ//[100]γ'', and spot 3 represents the [001]γ//[001]γ''.
Fig. 8(c)− 8(e) are the dark-field (DF) images obtained by employing
the superlattice locations marked (1−3) in Fig. 8(b), which show all
three disk-like variants of the γ'' phase. A part of the γ'' phase is
coarsened obviously when the aged time extends to 300 h, as illu­
strated in Fig. 8(f).

3.5. δ phase nucleation and growth

The morphologies of δ phase precipitation are presented in Figs. 9

and 10, revealing the distribution feature, growth process, and pre­
cipitation mechanism of the δ phase. Fig. 9 shows two modes of δ
phase nucleation and precipitation after aged at 750 °C for 100 h.
Fig. 9(a) depicts the first mode of phase precipitation, in which a small
amount of needle-like δ phase nucleates near the grain boundaries
and grows into the grain in a parallel relationship. The reason for the
first mode is that the precipitation of secondary carbides around grain
boundaries are rich in Cr and Mo to form regions rich in Ni and Nb
elements, thus promoting the precipitation of the δ phase.
The second mode of δ phase precipitation is transformed from
the metastable γ'' phase within the grains, as shown in Fig. 9(b) and
9(c). δ phase and metastable γ″ phase have the same atomic ar­
rangement on the close-packed plane [34] but different atomic
stacking sequences. The crystallographic and high-resolution trans­
mission electron microscopy (HRTEM) analyses confirm that the
transformation of γ″→δ is a pure geometric change of the compact
planes stacking sequence [31,35]. Due to the growth and coarsening
of the γ″ phase, a large lattice distortion generates between γ″ and γ
phases and a stacking fault appears on the compact plane (112) γ″,
turning the atomic stacking sequence from A1B1C1A2B2C2A1B1C1
into A1B1C1A2C1A2C2A1B1C1 [35,36]. The formation of consecutive
CA stacking sequences corresponds to the transformation of the D022
Fig. 8. (a) The TEM BF image showing γ'' phases after aged at 650 °C for 200 h. (b) stacking sequence to a locally δ phase D0a structure.
SAED pattern of (a) showing the existence of three γ'' phase variants. TEM DF images Fig. 10 shows the microstructure of the δ phase after aged at
from different variants: (c) [001]γ//[010]γ'', (d) [001]γ//[100]γ'', (e) [001]γ//[001]γ''. (f) 750 °C for 200–400 h. The volume fraction of needle-like δ phases
The TEM BF image showing γ'' phases after aged treatment at 650 °C for 300 h.
transformed from the γ'' phase within the grains increases

Fig. 9. Nucleation and precipitation methods of δ phase aged at 750 °C for 100 h.

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X. Liu, J. Fan, P. Zhang et al. Journal of Alloys and Compounds 930 (2023) 167522

Fig. 11. BF image, SAED pattern, and DF images of three variants of δ phase after aged
treatment at 750 °C for 300 h: (a) the BF image shows three different needle-like δ
phase variants. (b) SAED pattern and DF image of variation 1; (c) SAED pattern and DF
image of variation 2; (d) SAED pattern and DF image of variation 3.

and the tensile properties of Inconel 625 after the solution and
Fig. 10. Precipitation and growth of δ phase after aged treatment at 750 °C, SEM different aged treatments at RT are shown in Fig. 12 and Table 4,
micrograph of different aged time: (a, b) 200 h; (c, d) 300 h; (e, f) 400 h. respectively. The solid solution-treated alloy shows a YS of
∼366 MPa, a UTS of ∼811 MPa, and a fracture elongation of ∼73%. The
significantly after aged at 750 °C for 200 h, as shown in Fig. 10(a) and precipitation of the γ'' phase after aged at 650 °C for 200 h increases
10(b). In addition, the γ'' phase enriched region can also be found, the YS to ∼634 MPa and the UTS to ∼1050 MPa. Meanwhile, the
indicating the incomplete transition of the γ'' phase. Fig. 10(c)− 10(f) fracture elongation decreases to ∼42%. With the further increase of
reveal that the size and volume fraction of the δ phase continuously the aged time to 300 h and 400 h, the YS, UTS, and elongation of the
increase with the extension of the aged time to 300 h and 400 h. aged alloy have little change.
There is a competition between the δ phase precipitated near the Fig. 12(b) shows the representative engineering stress-strain
grain boundary and transformed from metastable γ'' phase within curves aged at 750 °C. The YS and UTS of the alloy increase slightly
the grains. The morphology of the δ phase is mainly intertwined as a while the elongation decreases slightly after aged treatment for
“basket-weave” shape inside the grains, as shown in Fig. 10(d) and 100 h. With the aged time extending to 300 h, the YS and UTS in­
10(f). The stability of the γ'' phase constantly decreases with the crease to 520 MPa and 945 MPa, respectively, and the fracture
increase of aged time. Therefore, the δ phase transformed from the elongation decreases to 46%. As listed in Table 4, the YS and UTS of
metastable γ'' phase is the predominant mode when the aged time the alloy after aged treatment at 650 °C are higher than those after
reaches 300 h and 400 h. aged treatment at 750 °C. Furthermore, the fracture elongation of the
The TEM observation was performed on the alloy aged at 750 °C alloy after aged treatment at 650 °C does not decrease significantly
for 300 h to characterize the variants of the δ phase. A typical BF compared with that after aged treatment at 750 °C. Therefore, the
micrograph with three distinct crystallographic orientations of aged treatment temperature for the Inconel 625 alloy should
needle-like phase is shown in Fig. 11(a). Three areas labeled 1, 2, and be 650 °C.
3 were selected for SAED patterns corresponding to the < 011 > γ The deformed substructures of the alloy are shown in Fig. 13,
zone axis of the matrix. The orientation relationship between the γ revealing the reasons for the difference in strengthening effects.
matrix and the δ phase was < 110 > γ//[100]δ, {111}γ//(020)δ. Among Many slip bands appear in the solution-treated sample after the
them, variant 1 conformed to the orientation relationship with the tensile test at RT, as illustrated in Fig. 13(a). The slip bands have been
matrix: [100]δ//[110]γ, (020)δ//(111)γ; variant 2 conformed [100]δ// confirmed to be situated on different {111} planes by comparing the
[101]γ, (020)δ //(111)γ; variant 3 conformed [100]δ//[011]γ, (020)δ// orientation of the slip bands with the diffraction vectors. Disloca­
(111)γ. The angles between the crystal orientation family < 110 > are tions slip freely on the {111} close-packed surfaces due to the lack of
60 °, suggesting that the angle between three different δ phase obstacles, which is related to the low tensile strength and high
variants is about 60 °. elongation [37]. The TEM image in Fig. 13(b) indicates that the
moving dislocations are pinned by dispersed γ'' phases after aged
3.6. Effect of secondary-phase precipitation on RT tensile deformation treatment at 650 °C for 300 h. The dislocation slipping is important
behaviors in coordinating the tensile deformation for the studied Inconel 625
alloy. The γ'' phases can effectively impede dislocation slipping by
The mechanical responses of the γ'' and δ strengthening effects the Orowan mechanism (relatively large particles) or cutting me­
were evaluated. The representative engineering stress-strain curves chanism (small particles) [13,38]. Consequently, the tensile

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X. Liu, J. Fan, P. Zhang et al. Journal of Alloys and Compounds 930 (2023) 167522

Fig. 12. Engineering stress-strain curves of the studied Inconel 625 alloy at RT: (a) specimens aged at 650 °C; (b) specimens aged at 750 °C.

Table 4
Tensile properties of Inconel 625 alloy evaluated at RT.

Heat treatment YS (MPa) UTS (MPa) EL (%)

Solution treated 365.5 ( ± 5.5) 810. 5( ± 4.6) 72.7 ( ± 0.4)

750 °C 50 h 390.9 ( ± 1.7) 851.4 ( ± 1.5) 64.4 ( ± 0.6)
750 °C 100 h 419.9 ( ± 2.1) 873 ( ± 3.5) 60.4 ( ± 0.7)
750 °C 200 h 462.8 ( ± 4.8) 903.5 ( ± 5.3) 60 ( ± 0.2)
750 °C 300 h 519.8 ( ± 4.7) 945.3 ( ± 10.4) 45.7 ( ± 1.4)
650 °C 200 h 633.5 ( ± 5.6) 1050.3 ( ± 5) 41.8 ( ± 1.6)
650 °C 300 h 629.1 ( ± 2.5) 1005.8 ( ± 0.6) 43.9 ( ± 1.2)
650 °C 400 h 640.6 ( ± 0.3) 1024.7 ( ± 2.8) 42.9 ( ± 1.2)

properties after aged treatment at 650 °C for 300 h have been sig­
nificantly improved.
As shown in Fig. 13(c) and (d), moving dislocations are tangled
around coarse needle-like δ phases after aged treatment at 750 °C for
300 h. The high-resolution TEM image of the interface between the
matrix (γ-Ni, FCC structure) and δ phase with an orthogonal D0a
structure is displayed in Fig. 13 (e). Based on the inverse fast Fourier
transform of the white box, interfacial dislocations (‘T′ symbol) exist
at the δ phases/matrix interface. The result confirms that the δ
phases/matrix interface is an incoherent interface, which is con­
sistent with a previous report on Inconel 718 alloy [39]. Due to the
severe lattice mismatch, lattice distortion regions should be around
the δ phases/matrix incoherent interfaces. The lattice distortion re­
gions can increase the resistance of dislocation slipping, thus
strengthening the alloy. Additionally, severe stress-concentration
areas appear between coarsened δ phases and the alloy matrix,
which provides some sites for the nucleation of microvoids. With the
increase of tensile strain in the non-uniform deformation stage, the
stress-concentration generated by dislocations accumulation ex­
ceeds the fracture stress of the matrix. As a result, many microvoids
appear around coarsened δ phases, as illustrated in Fig. 13 (f).
During plastic deformation, the YS of the alloy can be calculated Fig. 13. TEM bright-field image of the Inconel 625 alloy taken from fractured tensile
from the contribution of various strengthening mechanisms: solid specimens (a) solution treatment; (b) solution + 650 °C/300 h aged treatment; (c, d)
solution + 750 °C/300 h aged treatment; (e) typical HR-TEM image of the interface
solution hardening (σs), dislocation strengthening (σd), grain
between the matrix and δ phase in (d); (f) SEM micrographs from a near fracture area
boundary strengthening (σg), and precipitation strengthening (σp). showing many microvoids around δ phases.
The YS can be expressed as a summation of every individual con­
tribution [40]. contribution of σg is the same in aged samples. In addition, σs is
derived as follows.
σy = σ0 + σs + σd + σg + σp (1)

σ0 means the intrinsic strength or the so-called lattice fraction s = ki Cin

i (2)
stress, which is a basic parameter of the alloy [41].
In this study, all samples are fully recrystallized before aged where ki is the strengthening constant of solute i, Ci is the con­
treatment. The dislocation density and grain size of the aged sam­ centration solute i, and n = 1/2 is consistent with the dependence on
ples are consistent. Therefore, the σd can be ignored and the concentration in the Feltham equation [42]. Roth et al. [43]

8
X. Liu, J. Fan, P. Zhang et al. Journal of Alloys and Compounds 930 (2023) 167522

Table 5 around δ phase/matrix interfaces during the non-uniform de­

EDS results of the γ-matrix after aged treatment (at%). formation stage, which increases the tendency for microvoids
elements 650 °C/300 h 750 °C/300 h nucleation and expansion. The strengthening effect of δ phases is
Nb 1.7 ± 0.1 1.8 ± 0.1
weak compared with dispersed γ'' phases.
Cr 25.3 ± 0.2 25.3 ± 0.1
Mo 7.1 ± 0.1 7.2 ± 0.1 CRediT authorship contribution statement
Fe 4.7 ± 0.1 4.9 ± 0.1
Ti 0.2 0.2
Xudong Liu: Investigation, Writing – original draft, Visualization,
Al 0.4 ± 0.1 0.4 ± 0.1
Ni 60.7 ± 0.3 60.5 ± 0.2 Formal analysis, Data curation. Jiangkun Fan: Investigation, Writing
– original draft, Visualization, Formal analysis, Data curation.
Peizhe Zhang: Investigation, Methodology. Kai Cao: Investigation,
Methodology. Zixiao Wang: Investigation, Methodology.
calculated the main strengthening constant ki in nickel-based alloy Fulong Chen: Investigation, Methodology. Degui Liu: Investigation,
including Nb, Mo, Cr, Fe, Al, and Ti elements. EDS results of the γ- Methodology. Bin Tang: Data curation, Writing – review & editing.
matrix (more than 5 points) are statistically analyzed to study the Hongchao Kou: Data curation, Writing – review & editing.
change of the solute concentration after 650 °C/300 h and 750 °C/ Jinshan Li: Supervision, Funding acquisition.
300 h aged treatment. The statistical results are shown in the
Table 5. The solute concentration after aged treatment at 650 °C and Data Availability
750 °C for 300 h did not change significantly. Thus, the contribution
of σs to YS of the alloy is the same compared with 650 °C/300 h and All data are available from the corresponding author on reason­
750 °C/300 h aged treatments. able request.
For the samples subjected to different aged treatments, the
change in YS mainly comes from the difference in σp. The strength­ Declaration of Competing Interest
ening phases after 650 °C/300 h and 750 °C/300 h aged treatment are
γ″ and δ phases, respectively. Therefore, the difference in the The authors declare that they have no known competing fi­
strengthening effect between γ″ and δ phases (Δσp) can be estimated nancial interests or personal relationships that could have appeared
using Eq. (3): to influence the work reported in this paper.

Δσp= σp, γ″ -σp, δ = YS 650 °C/300 h – YS 750 °C/300 h (3) Acknowledgement

According to Eq. (3), the Δσp is about 109 MPa, thus the The authors gratefully acknowledge the National Science and
strengthening effect of the δ phase is weak compared with dispersed Technology Major Project (Nos. J2019-Ⅵ−0023–0140 and MJ-2018-
γ'' phases. G-48) and the Research Fund of the State Key Laboratory of
Solidification Processing (NPU) (No. 2022-TS-04) for the financial
4. Conclusions support of this work.

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