Journal of Materials Science & Technology 35 (2019) 1851–1859

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Research Article

Dynamic recrystallization behavior of GH4169G alloy during hot

compressive deformation
Dan Jia a,b , Wenru Sun b,∗ , Dongsheng Xu b , Fang Liu b
a
University of Chinese Academy of Sciences, Beijing, 100049, China
b
Institute of Metal Research, Chinese Academy of Sciences, Shenyang, 110016, China

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

Article history: The microstructure evolutions and nucleation mechanisms of GH4169 G alloy were studied by optical
Received 21 February 2019 microscope, electron backscatter diffraction (EBSD) and transmission electron microscope (TEM). The
Received in revised form 11 April 2019 hot compression tests were performed different imposed reductions in the range of true strain from
Accepted 12 April 2019
0.12 to 1.2 at the temperatures of 930 ◦ -1050 ◦ with strain rates of 0.01 s−1 -1 s−1 . It is found that cumu-
Available online 24 April 2019
lative and local misorientation increase firstly and then decrease when the strain is increased due to
the progress of dynamic recrystallization (DRX). The low angle boundaries (LAGBs) rapidly develop to
Keywords:
high angle boundaries (HAGBs) at relatively high deformation temperature or the low strain rate. There
GH4169G alloy
Dynamic recrystallization
are three DRX mechanisms observed for GH4169 G alloy during hot deformation. Discontinuous dynamic
Nucleation mechanism recrystallization (DDRX) as the dominant mechanism for GH4169 G alloy is characterized by typical neck-
lace structures and bulged-original boundaries. Besides, different deformation bands with dislocation
cells formed in deformed matrix at low temperature and large strain, which indicates that continuous
dynamic recrystallization (CDRX) contributed to the DRX process. The twin boundaries lost their coherent
characteristics and provide sites for nucleation, which also accelerates the nucleation of DRX.
© 2019 Published by Elsevier Ltd on behalf of The editorial office of Journal of Materials Science &
Technology.

1. Introduction microstructure evolution under different deformation conditions

for GH4169 G alloy. It is well known that dynamic recrystallization
GH4169 alloy has been widely used for hot section rotating (DRX) decreases the deformation resistance and yields beneficial
components of gas turbine aero-engine owing to its excellent fine grained structures resulting in better mechanical properties
mechanical and anticorrosion resistance at elevated temperatures and formability of alloys [8–10]. Some new dynamic recrystalliza-
up to 650 ◦ [1–3]. The emphasis on ever-increasing demand of tion kinetics model have been established which can well describe
stronger alloys has led to the development of superalloys. By micro- the DRX behavior [11,12]. In the past decades, the hot deforma-
alloying with phosphorus and boron, the stress rupture life and tion behaviors, as well as the DRX mechanisms of superalloy IN718
creep properties of GH4169 alloy can be improved significantly (GH4169) have been extensively studied [13–16]. However, the
[4,5], and the service temperature can be increased up to 680 ◦ . deformation process is quite complex and detail studies are needed
The new alloy added phosphorus and boron into the GH4169 com- to further investigate the nucleation mechanisms, especially about
position has been named as GH4169 G. the continuous dynamic recrystallization (CDRX) and twinning
The control of the thermo-mechanical processing is of great mechanisms. The information about the microstructure evolution
importance for the new alloy to obtain a superior performance. The during DRX of hot deformed GH4169 G alloy has been rarely investi-
processing parameters such as strain, strain rate and deformation gated experimentally. Besides, the microstructure evolution is well
temperature are all very important for controlling microstructure known to have a large impact on deformation behavior and the
of final products. Abnormal deformation conditions would induce deformation mechanisms vary with different superalloys. There-
surface cracks, inhomogeneous distribution of grain size and flow fore, further researches are needed.
localization [6,7]. Therefore, much attention should be paid to the In the present paper, the hot compression tests of GH4169 G
alloy have been conducted and the effects of deformation parame-
ter (strain, strain rate and temperature) on the evolutions of grain
∗ Corresponding author. microstructure are analyzed in detail. The nucleation mechanisms
E-mail address: [email protected] (W. Sun). for DRX correspond to certain condition have been demonstrated

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1852 D. Jia et al. / Journal of Materials Science & Technology 35 (2019) 1851–1859

using electron backscatter diffraction and transmission electron tion of misorientations is described in Fig. 1(b). The low angle grain
microscope. boundaries (LAGBs, 2◦ ≤ ␪<15◦ ) and high angle grain boundaries
(HAGBs,␪≥15◦ ) are defined. It should be noted that the major-
2. Materials and experimental procedure ity of the grain boundaries are HAGBs. Furthermore, it should be
mentioned that the fraction of 3 boundaries is about 48% in the
2.1. Materials specimen after solution treatment.

The master GH4169G alloy was prepared through vacuum 3.2. Microstructure evolution of hot deformation
induction melting followed by vacuum arc remelting and its chem-
ical compositions in weight percent are as following: Ni 52.65, Nb Fig. 2 demonstrates the microstructure evolution during the
5.20, Mo 3.12, Cr 18.77, Al 0.48, Ti 1.05, C 0.027, P 0.022, B 0.010, Fe deformation to a true strain of 1.2 under various conditions. The
balance. The ingot was cogged and hot close-die forged into a cake- microstructures are significantly affected by deformation temper-
like forging after a homogenization treatment. The specimens used ature and strain rate. As shown in Fig. 2(a), (b) and (c), the initial
in this paper were cut from the cake-like GH4169 G forging and equiaxed grains are replaced by a microstructure composed of the
soaked at 1020 ◦ for 1 h to ensure the uniformity of microstructure elongated grains and some fine new recrystallized grains formed at
for all the specimens. the grain boundaries when the deformation temperature is 950 ◦ ,
which exhibits the typical partial DRX microstructure. In addition,
the fraction of the elongated grains increases with the increas-
2.2. Hot compression tests
ing strain rate. It is apparent that the increasing of the strain rate
restricts the DRX of the alloy. Fig. 2(d) and e show that the ini-
Isothermal hot compression tests were carried out on Gleeble
tial large grains were completely replaced by the uniform and fine
3500 thermo-mechanical simulator to evaluate the microstructure
DRX grains when the deformation temperature is 1000 ◦ . How-
evolution during hot working under the temperature range from
ever, the elongated grains were observed when the strain rate is
930 ◦ to 1050 ◦ and strain rate 0.01 s−1 , 0.1 s−1 and 1 s−1 . Cylindri-
up to 1 s−1 as shown in Fig. 2(f). When the deformation temper-
cal specimens with 10 mm in diameter and 15 mm in height were
ature was increased up to 1050 ◦ , the grain microstructures were
prepared. Graphite was used as lubricant between specimen and
characterized by the complete DRX, as shown in Fig. 2(g), (h) and
compression dies in order to reduce the friction. The specimens
(i). Meanwhile, the average grain size decreased gradually with the
were heated to preset temperature at a rate of 10 ◦ /s and soaked
increasing strain rate.
at the temperature for 5 min before compressed to various strains,
and then were immediately quenched by water to preserve the
3.3. The effect of strain on dynamic recrystallization
deformation microstructure.
In order to understand the effects of true strain on microstruc-
2.3. Microstructure analysis ture evolution during dynamic recrystallization, the hot compres-
sion tests with different final true strains of 0.12, 0.35, 0.69, and
The deformed specimens were sliced along the compression axis 1.2 were carried out respectively. Fig. 3 illustrates the influence
for microstructure observation. The cutting surfaces were mechan- of true strain on orientation imaging microscopy (OIM) maps at
ically polished and etched electrolytically with a solution consisting 990 ◦ and 0.1 s−1 . Obviously, the grain microstructures are sig-
of 10 g oxalic acid in 90 ml water at an applied potential voltage nificantly affected by true strain. The grain boundaries become
of 6 v for 6–9 s. Grain boundary can be deeply etched using this serrated and there is almost no DRX grains, which the strain up
method, making the grain size easily measurable. Due to the hetero- to 0.12 is measured (Fig. 3(a)). It is commonly known that the ser-
geneity of deformation during hot compression, the microstructure rated grain boundaries retain high strain gradient, and become the
observations were focused on the central part of the specimens. For prior sites for the nucleation of DRX grains [2]. As the strain increas-
electron backscatter diffraction (EBSD) observation, the specimens ing to 0.35, the typical necklace structures are observed as shown
were mechanically polished and followed by electropolishing in in Fig. 3(b), some fine new dynamically recrystallized grains are
a solution of 10% perchloric acid in ethanol at 30 V. Microstruc- to be distributed irregularly along the prior grain boundaries. This
ture analysis was carried out using a fully automated EBSD system indicates that the grain boundaries are the preferential sources for
with channel 5 software. Depending on specific grain size, measure- the initiation of new grains. With the further straining (␧ = 0.69),
ments were performed over two types of areas using the following the DRX grains become more prevalent, as illustrated in Fig. 3(c).
parameters: a spot size of 6.0, accelerating voltage 20 kV, and a step After reaching the strain of 1.2, DRX takes place in most of the area
size with 0.14 ␮m. The information such as grain boundary char- and the grains are refined significantly as plotted in Fig. 3(d). It is
acteristics was obtained accurately by using the EBSD technique. apparent that the DRX is promoted by the increasing strain.
In addition, dislocation and recrystallization were examined using The effects of strain on the orientation gradient are studied by
transmission electron microscope (TEM) on a JEOL 2010 TEM oper- carrying out misorientation analysis. The point to origin (cumula-
ated at 200 kV. Thin foils for TEM observation were prepared by tive) misorientation and point to point (local) misorientation are
mechanically grinding specimen slices to 50 ␮m thick and twin-jet calculated along the lines marked in Fig. 3. Both the cumulative
electropolishing in a mixture of 90% alcohol and 10% perchloric acid misorientation and local misorientation along grain boundaries
at -20 ◦ under voltage of 24 V. (line A1) are less than 5◦ as plotted in Fig. 4(a). Meanwhile, the
cumulative misorientation from grain boundary to grain interior
3. Results does not exceed 11◦ (Fig. 4(b)), indicating the development of
misorientation accumulates. LAGBs lower than 10◦ are considered
3.1. Initial microstructure to be necessary for nucleation of DRX [6]. The results imply that
LAGBs are accumulated on the vicinity of initial grain boundaries
Fig. 1(a) presents the microstructure of the GH4169 G alloy prior under relatively low strain 0.12 at 990 ◦ , where the strain energy is
to hot deformation. It can be found that the initial microstructure not sufficient for the nucleation of DRX grain. The misorientation
mainly consists of equiaxed grains with an average size of 73␮m profiles along the lines B1 and B2 at true strain of 0.35 are shown in
and lamella-like straight annealing twins. In addition, the distribu- Fig. 4(c) and d. It is clearly seen that the point-to-origin misorienta-
 D. Jia et al. / Journal of Materials Science & Technology 35 (2019) 1851–1859 1853

◦
Fig. 1. Microstructure of the GH4169 G specimens soaked at 1020 for 1 h prior to hot compression: (a) orientation image microscopy map; and (b) misorientation angle
distribution.

Fig. 2. Optical micrographs of GH4169 G alloy deformed to 1.2 true strain at different temperatures with various strain rates.

tion can easily exceed 20◦ both along the grain boundary and grain the two main misorientation jumps appear at the distance range
interior, where the boundaries of growing nuclei can accumulate of 20-30␮m along the grain boundaries (Fig. 3(e)), while there are
adequate misorientation to become HAGBs. This suggests that the obvious misorientation jumps located at about 11␮m and 18␮m
misorientation accumulates and the progressive lattice rotation from the origin, which implies the misorientation of about 8-12◦ .
has been developed corresponds to the lower strain, which would These jumps indicate that the original grains can be subdivided by
accelerate of DRX. Fig. 4(e) and f show that the local misorienta- different orientation bands when deformed to true strain of 0.69.
tions do not monotonically increase with the increase of distance It is widely accepted that the continuous dynamic recrystallization
along the grain boundaries and grain interior. Fig. 4(f) shows that (CDRX) nucleation mechanism is characterized by progressive sub-
1854 D. Jia et al. / Journal of Materials Science & Technology 35 (2019) 1851–1859

Fig. 3. OIM maps of specimens deformed to different of strains under conditions of 990 ◦ and 0.1 s−1 : (a) 0.12; (b) 0.35; (c) 0.69; and (d) 1.2.

grain rotation, and 10-15◦ misorientation angles often indicate the for grain boundary migration, which facilitates the development
occurrence of CDRX in subgrain substructures [8]. From Fig. 4(e) of DRX process. From the Fig. 6(c) and d, the cumulative misori-
and f, the local misorientation across the original grain boundaries entations are lower than 10◦ and the misorientation from grain
are 10-15◦ under 0.69 strain, implying that CDRX really occur in boundaries to grain interior are less than 6◦ . These results indicate
a localization way in GH4169 G during hot deformation. As shown that a significant fraction of subgrains are obtained under the strain
in Fig. 4(g) and h, the cumulative misorientation significantly rate of 1 s−1 , where the DRX process is limited.
decreases to a level lower than 2◦ when true strain reaches 1.2, Fig. 7 depicts the OIM maps and misorientation angle distribu-
indicating that the deformed grains are replaced by the DRX grains tion of the specimens deformed at 950 ◦ and 1000 ◦ . Here, the true
with low dislocation density, which is in a good agreement with strain and strain rate are 1.2 and 0.1 s−1 . HAGBs and LAGBs are rep-
the grain microstructure shown in Fig. 3(d). resented by black lines and gray lines, respectively. It can be found
that a majority of grains are elongated with a high density of LAGBs
3.4. The effects of strain rate and temperature on dynamic and some DRX grains appear at the initial original grain boundaries
recrystallization (Fig. 7(a)). The LAGBs are inherently associated with the substruc-
tures and dislocations, which would be developed into HAGBs and
Fig. 5 shows the effects of strain rate on the microstructure accompany with the DRX initiation. As shown in Fig. 7(b), the frac-
evolution of GH4169 G. Here, the deformation temperature and tion of LAGBs is about 70.8%, which implies that the dislocation
strain are 1000 ◦ and 0.35, respectively. For the specimen deformed annihilation and rearrangement are hindered under the relatively
at strain rate of 0.01 s−1 , a large amount of refined DRX grains low deformation temperature. When the temperature increases to
can be found along the deformed grain boundaries. With the 1000 ◦ , the initial large grains almost disappear and notable refined
increase of strain rate, DRX becomes difficult to occur and the DRX DRX grains are formed, as illustrated in Fig. 7(c). Meanwhile, it can
degree obviously decreases. This is because that high strain rate be found that the fraction of LAGBs decreases to 24.5%, which is
provides less time for the movements of dislocations and grain significantly affected by the transformation from LAGBs to HAGBs
boundaries. Therefore, the nucleation and growth of DRX grain is at higher deformation temperature (Fig. 7(d)). Furthermore, it can
postponed. be found that both the DRX degree and DRX grains size increase
Fig. 6 illustrates the point to point misorientation and the point with the increasing deformation temperature. This is because the
to origin misorientation along the lines which marked in Fig. 5. It is nucleation of DRX grain is mainly induced by dislocation evolu-
seen that the local and cumulative misorientation are sensitive to tions such as generation, interaction and annihilation, which are
strain rate. As shown in Fig. 6(a) and (b), the cumulative misorienta- thermally-activation process. On the other hand, the growth of DRX
tion can easily exceed 15◦ both near the original grain boundaries grains is closely related to grain boundary migration. Both dislo-
and within the grains, implying that some of the developed sub- cation evolution and grain boundary migration become more and
grains have been transformed into HAGBs. It is well known that high more intense with the increased deformation temperature due to
orientation gradients and dislocation density are essential for the the high driving force. Thus, the DRX process can be accelerated
nucleation of DRX [17]. The lower strain rate can provide more time under the relatively high deformation temperature [2,6].
 D. Jia et al. / Journal of Materials Science & Technology 35 (2019) 1851–1859 1855

Fig. 4. Misorientation angle along the lines marked in Fig. 3: (a) A1; (b) A2; (c) B1; (d) B2; (e) C1; (f) C2; (g) D1; (h) D2.
1856 D. Jia et al. / Journal of Materials Science & Technology 35 (2019) 1851–1859

Fig. 5. OIM maps of GH4169 G deformed to a true strain of 0.35 at 1000 ◦ and strain rates of (a) 0.01 s−1 and (b) 1 s−1 .

Fig. 6. Misorientation angle along the lines marked in Fig. 5: (a) E1; (b) E2; (c) F1; (d) F2.

4. Discussion tion densities on the two sides of the grain boundary, serve as the
sources for the local bulging from the initial grain boundary [18].
4.1. Bulging of the initial grain boundaries Subsequently, these subgrain boundaries further transform into
HAGBs of DRX nuclei through the local grain boundaries bulging.
Fig. 8 shows the TEM micrograph for the GH4169 G alloy Therefore, the bulging of prior grain boundaries becomes the pri-
deformed at the 990 ◦ and 0.1 s−1 to the true strains of 0.12 and 0.35. ority sites for nucleation of DRX grains [13,19,20]. With the strain
It is revealed from Fig. 8(a) that numerous dislocation networks further increasing up to 0.35, new DRX grains with low dislo-
as well as the regularly-arranged dislocations indicate that the cation density can be observed in Fig. 8(b). This is attributed to
heterogeneous distribution of dislocations under relatively small the deformation storage energy increases as the strain increased,
deformation degree (␧ = 0.12). In order to reduce the stress con- which brings the strong driven force for the movements of dis-
centration, the piled up dislocations rearrange themselves near the location and grain boundary. Due to the elimination of a large
grain boundary and form low angle subgrain boundaries, leading number of dislocations during the nucleation process, the dis-
to the occurrence of the LAGBs. Fig. 4(a) and (b) demonstrated location density in the dynamic recrystallization nucleus is very
that the fraction of subgrains with LAGBs was relatively higher low. As stated above and noted that the emergence of such grain
at lower strain. Since the large difference between the disloca- boundary morphology confirms that the nucleation mechanism of
 D. Jia et al. / Journal of Materials Science & Technology 35 (2019) 1851–1859 1857

Fig. 7. OIM maps and misorientation distribution of specimens deformed at 0.1s−1 to a true strain of 1.2: (a) and (b) 950 ◦ ; (c) and (d) 1000 ◦ .

Fig. 8. TEM micrographs of GH4169 G deformed at 990 ◦ and 0.1 s−1 at true strains of: (a) 0.12 and (b) 0.35.

GH4169 G alloy belongs to discontinuous dynamic recrystallization that formed by deformation (marked by frame in A), leading to
(DDRX). division of grain into different orientation. A close-up view which
marked by frame in B indicates that some dislocation cells with
4.2. Progressive subgrain rotation disordering network structure developed the band (Marked with
circle in Fig. 9(c)). This structural response on hot deformation
The nucleation mechanisms of CDRX nucleation occurred simul- which formed by strain-induced boundaries when large strain gra-
taneously in Ni based superalloy [2,13]. Nucleation by subgrain dients implemented [22,23], leading to the evolution of strain
rotation usually propelled in the interior or the boundary of induced LAGBs. Most mobile dislocations are trapped by subgrain
grain [21]. The deformed bands are observed within the grains boundaries, resulting in an increase in their misorientations and
as the specimen deformed upon a true strain of 0.69 at 990 ◦ , gradual transformation into HAGBs [24]. The large orientation gra-
as shown in Fig. 9(a). From Fig. 9(b), a great deal of dislocations dients both along the grain boundary and within the grain are
1858 D. Jia et al. / Journal of Materials Science & Technology 35 (2019) 1851–1859

Fig. 9. TEM micrographs show the deformed bands upon a true strain of 0.69 at 990 ◦ /0.1 s−1 .

only considered as an assistant nucleation mechanism of DRX for

GH4169 G alloy.

4.3. Twin boundary

As shown in Fig. 11(a), the annealing twins can acceler-

ate boundary bulging and lead eventually to the growth of a
dislocation-free zone that acts as DRX nuclei, indicating twin
boundary plays an important role in the nucleation mechanism
of DRX for GH4169 G alloy during hot deformation. The exis-
tence of boundaries can help and even accelerate the serration
of grain boundaries and separation of bulged portion from the
pre-existing grains, thereby facilitating DRX [25,26]. Moreover, it
can be found from Fig. 11(b) that there are some dislocations
pile-ups near the twin boundaries and the main dislocation sub-
structures are subgrains, which are effective in the nucleation
of DRX grains within grain. Generally, the coherent twin bound-
aries are energetically less favorable to act as nucleation sites
Fig. 10. The fraction of different misorientation angle for GH4169 G alloy deformed due to lower interface energy. However, the original twin bound-
to various strains at 990 ◦ and 0.1 s−1 .
aries lost their coherent characteristics during hot deformation
owing to the crystal rotation. The twin boundaries would trans-
form into considerable mobile boundaries [27], which provide
presented in Fig. 4(e) and (f), which confirm that the mecha- position for the DRX nucleation within grain. The local misori-
nisms of CDRX take place during hot deformation of GH4169 G entation is imaged by Kernel Average Misorientation mapping
alloy. In general, the fraction of misorientation between 10-15◦ (KAM) in Fig. 12, which used as a measurement of the intra-
directly responses the effect of CDRX during hot deformation [13]. granular misorientation. The misorientations between subgrains
Fig. 10 summarized the fraction of different misorientation angle are typically of the order of 0-5◦ . The new recrystallized grains
for GH4169 G alloy deformed to various strains at 990 ◦ and 0.1 with lower dislocation density (blue color) at the twin boundaries
s−1 . It can be seen that the fraction of grain boundaries with 10- existing in the initial grains are observed in the specimen which
15◦ misorientation can hardly exceed 2%, indicating that CRDX deformed to a true strain of 0.35 under conditions of 1000 ◦ and
 D. Jia et al. / Journal of Materials Science & Technology 35 (2019) 1851–1859 1859

Fig. 11. TEM morphologies of the nucleation at twin boundaries at true strain of 0.12 under the condition of 1000 ◦ /0.1 s−1 .

(3) The deformation bands with dislocation cells were found in the
interior of the grain at low temperature and large strain which
confirmed the CDRX mechanism also occurred in GH4169 G
alloy, while the progressive subgrain rotation is considered as
an assistant nucleation mechanism of DRX due to the small
fraction of grain boundaries with 10-15◦ .
(4) Twinning boundaries were observed to accelerate the grain
boundary bulging and lose their coherent characteristic to pro-
vide sites for nucleation, which are beneficial to the nucleation
of GH4169 G alloy.

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