Progress in Natural Science: Materials International 33 (2023) 232–243

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Progress in Natural Science: Materials International

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Effect of carbon addition on microstructure and mechanical properties of a

typical hard-to-deform Ni-base superalloy
Lei Jia a, Heng Cui a, **, Shufeng Yang b, *, Shaomin Lv c, d, Xingfei Xie c, d, Jinglong Qu c, d
a
Collaborative Innovation Center of Steel Technology, University of Science and Technology Beijing, Beijing, 100083, China
b
State Key Laboratory of Advanced Metallurgy, University of Science and Technology Beijing, Beijing, 100083, China
c
Beijing GAONA Materials & Technology Co., Ltd., Beijing, 100081, China
d
High-Temperature Materials Institute, Central Iron and Steel Research Institute, Beijing, 100081, China

A R T I C L E I N F O A B S T R A C T

Keywords: In this paper, the as-cast microstructure, microsegregation, and mechanical properties of GH4151 superalloys
GH4151 superalloys with a carbon addition were studied by scanner electron microscopy (SEM), transmission electron microscope
Carbon (TEM), electron probe microanalysis (EPMA), differential thermal analyzer (DSC), and electron backscattered
Microstructure and microsegregation
diffraction (EBSD). The results show that the solid solution effect of carbon in alloys is limited, the addition of C
Mechanical properties
from 0.01 to 0.08 wt% significantly refines the secondary dendrite spacing(SDAS) from 61.7 to 57.4 and 51.8 μm.
Due to the influence of thermal solutal convection, the most severe segregation is found in the C-0.04 alloy, and
the solidification ranges of C-0.01, C-0.04, and C-0.08 alloys are 87
C, 96
C, and 83
C, respectively. Owing to
the reduced solidification pores and formed finely dispersed carbides, C-0.04 shows excellent ultimate tensile
strength (442 MPa) and superior total elongation (1.368%) at 1100
C much better than that of C-0.01(130.7
MPa, 0.085%) and C-0.08(248 MPa, 1.026%).

1. Introduction region for γ. Therefore, it is difficult to maintain the temperature

within the single-phase region of γ during the hot working process of
Aviation technology has progressed towards a larger scale, higher GH4151 high-temperature alloy, especially during the cogging process.
thrust-weight ratios, and increased efficiency in aero-engines [1,2]. As a On the other hand, if the deformation temperature is within the dual-
result, nickel-based superalloys have become a popular choice due to phase region of γþγ0 , a high proportion of fine and dispersed γ0 parti-
their superior mechanical properties and ability to resist oxidation at cles can effectively suppress the migration of dislocations and grain
high temperatures [3,4]. A reliable technique to enhance the perfor- boundaries, thereby significantly improving the alloy's resistance to hot
mance of nickel-based superalloys for higher temperature service in- deformation. Additionally, adding many elements results in the
volves adjusting and augmenting the amounts of strengthening extremely high crack susceptibility of alloys [9,10]. This is because the
phase-forming elements, including Al, Ti, and Nb, as well as addition of large amounts of Al, Ti, and Nb elements would lead to the
solution-strengthening elements such as W, Co, Cr, and Mo [5,6]. expansion of the freezing range of the alloy [11] and result in the pre-
GH4151 alloy is a typical representative of deformed high-temperature cipitation of numerous brittle intermetallic phases like MC carbide, Laves
alloys in service above 800
C [7], and the γ0 phase content is up to phase and (γþγ0 ) phase in the interdendritic [12,13]. The wide freezing
55% [8]. The combination of age-precipitation strengthening elements range and severe segregation lead to insufficient replenishment in the
Al, Ti, and Nb exceeds 10 wt% [9], and the refractory elements W, Mo, semi-solid stage [14,15], which reduces the denseness and homogeneity
Cr, and Co exceed 34 wt%, which is a typical hard-to-deform Ni-base of both microstructure and composition of alloys [16], deteriorating the
superalloy for serves above 800
C. mechanical properties of the alloy and results in the formation of hot
However, the high degree of alloying results in a significant increase tearing during industrial production. While the elimination of cracks by
in the dissolution temperature of the γ0 phase and a decrease in the sol- parameter optimization often requires higher production costs, e.g.,
idus temperature of the γ matrix, leading to a very narrow single-phase increasing the ingot mold preheating temperature and thermal

* Corresponding author.
** Corresponding author.
E-mail addresses: cuiheng@ustb.edu.cn (H. Cui), yangshufeng@ustb.edu.cn (S. Yang).

https://doi.org/10.1016/j.pnsc.2023.05.008
Received 23 March 2023; Received in revised form 18 May 2023; Accepted 22 May 2023
Available online 9 June 2023
1002-0071/© 2023 Chinese Materials Research Society. Published by Elsevier B.V. This is an open access article under the CC BY-NC-ND license (http://
creativecommons.org/licenses/by-nc-nd/4.0/).
L. Jia et al. Progress in Natural Science: Materials International 33 (2023) 232–243

annealing, etc. [17,18]. microstructure morphology of the alloy was observed by a field-emission
The micro-element carbon has a great influence on the solidification scanning electron microscope (FE-SEM, Hitachi JSM-6701F) equipped
characteristics and mechanical properties of nickel-based superalloys with an energy-dispersive spectrometer (EDS, Aztec Xmax 50 X). To
[19]. Adjustment of the carbon content in actual industrial production is determine the chemical segregation and compositions of precipitated
also easy to achieve. Although a great deal of investigation has been done phases, a semi-quantitative measure was obtained using an electronic
on the role of carbon in superalloys, it is still controversial so far [20-22]. probe microscope analyzer(EPMA-1720H). Quantitative determination
With the increase of carbon addition, the segregation of rare earth, of the composition at four positions was done in dendritic cores, inter-
tungsten, and tantalum in nickel-based superalloys is significantly dendritic regions, and precipitated phases. In addition, the crystal
reduced, and the formation of (γþγ0 ) eutectic is limited [23]. Nonethe- structures of the interdendritic precipitations were determined by
less, excessive carbon content can result in the precipitation of script-like transmission electron microscope(TEM), and the specimens for TEM
or elongated MC carbides, which can initiate cracks at the carbide/matrix were prepared by cutting the samples into slices with a thickness of 500
interface and ultimately weaken the mechanical properties [9,22]. The μm. Mechanically ground to 60 μm thickness and punched into circular
carbon content in conventional deformed Ni-based superalloys is usually slices with a radius of 3 mm. The twin-jet electro-polishing was per-
below 0.2 wt % to prevent the deleterious effects of coarse MC primary formed in a solution of 10% HClO4 þ 90% CH3CH2OH at 20
C, and 24 V.
carbides on ductility and creep properties [24]. TEM observations were performed with a Talos F200x G2 transmission
However, for GH4151 alloy the C content in the nominal composition electron microscope (Thermo Fisher, Waltham, MA, USA) operated at
is designed to be between 0.04–0.08 wt%, and the wide control of the 200 kV. The electron backscattered diffraction (EBSD, Aztec) samples
composition range causes a great deal of trouble for the current industrial were electropolished with 20 ml H2SO4 þ 80 ml CH3OH at 10–20 V for
production. Moreover, the main carbide forming elements Ti, Nb, and W, 10–15 s, and the grain size was scanned via EBSD at a step size of 5 μm.
Mo are all added in the GH4151, which will inevitably bring a large The scanning results were then analyzed and characterized by using HKL-
impact on the microstructure and mechanical properties of the alloy. Channel 5 software.
Therefore, it is necessary to study the control range of carbon in nickel-
based forged superalloy GH4151 alloy with high Al, Ti, and Nb con-
2.3. DSC analysis
tents, to build the foundation for optimizing the C content in GH4151
superalloy and producing crack-free highly alloyed ingots with no crack
The freezing range and the transition temperature of the intermetallic
defects. In this paper, the as-cast microstructures, segregation behavior,
phase were measured by differential scanning calorimetry (DSC). The
precipitates, and mechanical properties of nickel-based forged superal-
specimen size was Φ5  0.3 mm, the heating rate was 10
C/min, and the
loys with different carbon contents prepared by vacuum induction
test temperature range was 1100–1400
C. In addition, the heating curve
melting (VIM) were studied by SEM, TEM, EPMA, DSC, and EBSD.
of the empty crucible was used as the baseline before the experiment, and
the experimental curve was obtained by subtracting the baseline from the
2. Experimental
heating curve of the sample and the crucible as the heating curve of the
piece.
2.1. Materials production

GH4151 alloys with different carbon contents (0.01, 0.04, and 0.08 2.4. Mechanical property analysis
wt%) were prepared in a 25 kg vacuum induction melting (VIM) furnace.
The Standard chemical compositions of GH4151 alloy are shown in The hot-cracking susceptibility is approximately related to the high-
Table 1. Electrolytic C, Ni, Co, Cr, Mo, W, and other high-purity raw temperature toughness corresponding to solidus temperatures below
materials (purity >99.9%) are first added to the furnace and then vac- 150
C and 100
C of the nickel-based alloys [25]. Therefore, the tensile
uumed to below 0.1 Pa before increasing the power for melting. To avoid tests of the as-cast GH4151 alloy were evaluated by a Gleeble-3800
gas pollution, the materials of Al, Ti, Zr, and Nb are added in the last. The thermal simulation testing machine at 1100
C and a constant strain
refining temperature and refining time were kept at 1600  50
C and rate is 1/s1. The size of sample size is Φ 6  116.5 mm, and the gauge
102min. The pouring temperature was 1470  10
C. The uniform distance is 12 mm was cut from the R/2 of the ingot. The schematic di-
liquid metal was poured into the cast iron mold to obtain three ingots of agram of the tensile specimen is presented in Fig. 1. The number of
Φ100  300 mm. The chemical composition and interstitial elements of tensile specimens for each alloy is three times to obtain the average
ingot were analyzed by inductively coupled plasma atomic emission value. Yield strength (σ 0.2), Ultimate tensile strength (σ b), and fracture
spectrometry (ICP-OES, GB/T 30902-2014, China), carbon sulfur elongation (δ) are shown in Table 3. The tensile fracture of the sample
analyzer (EMA-920V2, HORIBA), and oxygen nitrogen analyzer (EMGA- was examined under the scanning electron microscope for deformation
830, HORIBA), respectively, and the results are presented in Table 2. observation. In addition, the hardness of the alloys was measured using a
Vickers hardness tester with a load of 500 g and a duration time of 15 s.
At least ten measurements were conducted to obtain the averaged values.
2.2. Microscopy and microstructural analysis

The samples with a size of 15  15  15 mm were cut from the half 2.5. Thermodynamic calculation
radius (1/2R) and half height (1/2H) of the ingot, using the standard
metallographic technique to get a mirror surface, then etched with a The chemical information and the solidification path were calculated
solution of 0.5g CuCl2þ10 ml C2H5Oþ10 ml HCl for 3~10s to observe by the Thermo-Calc software using the TTNi8 database. The simulated
microstructure. The γ0 phase was observed by electrochemical erosion temperature range was set to 200–1400
C, and the results were returned
with 2.4 ml H3PO4 þ 8 ml HNO3 þ 10 ml H2SO4 at 5–6 V for 6–10 s. The at 10
C intervals until a part of the liquid was 0.02.

Table 1
Standard chemical compositions of GH4151 alloy (wt. %).
Elements C Cr Al Ti Mo Nb W

Composition 0.04–0.08 10.0–12.0 3.5–4.0 2.5–3.1 4.0–5.0 3.0–3.5 2.5–3.5

Elements Co V Ni O N B Zr
Composition 14.0–16.1 0.4–0.8 Bal. 0.0020 0.0030 0.010 0.05

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Table 2
Chemical composition of the samples (wt. %).
Ingot C Cr Al Ti Mo Nb W Co V Ni O N

#1 0.011 11.05 3.81 2.85 4.62 3.35 3.14 15.05 0.62 Bal. 0.0012 0.0022
#2 0.042 11.08 3.72 2.81 4.53 3.28 3.21 15.12 0.67 Bal. 0.0010 0.0020
#3 0.078 11.15 3.84 2.78 4.61 3.31 3.17 15.08 0.61 Bal. 0.0007 0.0018

C (12.06 wt %), Nb, and Ti, indicating that they are MC carbides.
Another important point to note is the formation of distinct Moir
e
patterns around the precipitate phase. This phenomenon is caused by the
lattice distortion resulting from the formation of the precipitate phase.
Such distortion induces interference and diffraction of light, creating a
series of alternating bright and dark textures. The crystal structure of the
sunflower-like phase(Fig. 3c) is face-centered cubic, rich in Al and Ti
elements, with a parameter of a  0.346 nm, which is consistent with the
structural features of γ and γ0 see in Fig. 3d [26], indicating that it is
eutectic γþγ0 phase. The large size eutectic phase γþγ0 precipitates at a
Fig. 1. Schematic diagram of the tensile specimen. higher solidification temperature, which is not conducive to the feeding
shrinkage of the molten alloy and deteriorates its fluidity [27]. Addi-
3. Results tionally, the presence of residual liquid phases during the final stage of
solidification results in a point contact between adjacent solid dendrites,
3.1. Microstructure characteristics without achieving a true dendrite connection, making it prone to
cracking, see in Fig. 3c. From Fig. 3d, it can be observed that dislocations
Fig. 2a-e shows typical dendrite morphologies for different carbon are mainly concentrated in the γ matrix and form some slip bands. The
contents. Among them, the dark black region is the dendrite (DR), and entangled dislocations in the γ channel indicate that the matrix is the
the bright area is the interdendritic (ID). Table 3 shows that secondary main deformation zone [28]. Moreover, dislocations move within the
dendrite arm spacings (SDAS) were measured from these images. It can lattice of the γ0 phase, resulting in a displacement or shear of the crystal
be seen that the addition of carbon has shown a significant effect on structure. This leads to stacking fault shear, which can enhance the ma-
secondary dendrite arm spacing(SDAS), as the increase of C content from terial's strength and high-temperature resistance.
0.1 to 0.40 and 0.08 wt% significantly decreased from 61.7 to 57.4 and In addition, Fig. 4 presents the EBSD images of the alloys with
51.8 μm. different carbon contents. It can be seen that the grain structure of the
Fig. 2f-h shows a high-magnification microstructure of different car- alloy is coarse and uneven during the solidification of conventional metal
bon addition detected by back-scattered electrons (BSE). It can be seen molds [29]. Moreover, with the addition of carbon, the grain size of the
that the gray and coarse phase (marked phase A), gray and slaty phase alloy decreased (Fig. 4a–c). The smallest grain size of the alloy was
(marked phase B), white and blocky phase (marked phase C), and gray observed at 0.08 wt% carbon(Fig. 4c). Meanwhile, the {100} EBSD pole
and angular phase (marked phase D) precipitate in the interdendritic figures of the different carbon content alloys are shown in Fig. 4(a')-(c').
region. The quantitative chemical composition of precipitates was In the C-0.01 alloys, the maximum uniform density of the alloy is 38.4
analyzed by EPMA and is shown in Table 4. For phase A, the atomic ratio (Fig. 4(a')). At carbon contents of 0.04 and 0.08 wt%, the texture density
of Ni to (Al þ Ti) is ~3 and the element characteristic is similar to that of decreases to 33.3 and 27.4, respectively, as shown in Fig. 4(b') and 4(c').
γ0 phase, indicating it is (γþγ0 ) eutectic phase. The slate-like phase B is Texture weakening resulted from grain refinement caused by increased
rich in Nb and Ti elements, and the mass percentage of Ti elements is nucleation rate during solidification [30].
higher than that of Al elements, indicating it is the η phase. Furthermore,
phase C is distributed on both sides of phase B, and the elements enriched 3.2. Dendritic segregation
in phase C are mainly Mo, Co, Cr, and Nb while depleted in Al and Ti,
which should be Laves phase [17]. Finally, the atomic ratio of C to (Nb þ To figure out the effects of C on the degree of element segregation at
Ti) in phase D is ~1, indicating it is MC carbide. the dendrite arm and interdendritic region were detected by EPMA, and
Next, the effect of carbon addition on precipitation is further dis- the elemental segregation coefficient k (defined as the ratio of element
cussed. The precipitation phase types of alloy C-0.01 (Fig. 2f) and alloy C- content of dendrite arms to the interdendritic elemental content) was
0.04 (Fig. 2g) are similar, while in alloy C-0.04, the size of the slate-like calculated. For the negative element (k > 1), indicating the degree of
phase was increased from 25 μm to 60 μm, and the number of white element segregation to the dendritic arm. For the positive element (k <
precipitated phase significantly increased. The morphology of the white 1), the degree of element segregation to the interdendritic region. The
precipitated phase changed from small blocky to lamellar. In addition, results are shown in Fig. 5a. It can be seen that for the alloy C-0.04,
the blocky phase(marked phase D) begin to appear in the interdendritic positive segregation elements Nb (kNb ¼ 0.306), Ti (kTi ¼ 0.462), Al
regions(Fig. 2h). When the carbon content was increased to 0.08 wt%, (kAl ¼ 0.792), and Mo (kMo ¼ 0.945) segregate to the interdendritic
except for phase D, the other phases precipitated are difficult to appear in regions; negative segregation elements W (kW ¼ 1.459), Cr (kCr ¼
the as-cast structure (Fig. 2, f). Additional TEM bright-field images and 1.141), and Co (kCo ¼ 1.136) segregate to the dendritic cores; and Ni
selected regions' diffraction pattern analysis were used to determine the (kNi ¼ 1.003) does not show any obvious segregation. However, the
structure of that precipitated phase, as shown in Fig. 3. The crystal addition of 0.080 wt% C decreases the segregation of Nb (kNb ¼
structure of the white precipitated phase(Fig. 3a) is hexagonal with pa- 0.306–0.499), Ti (kTi ¼ 0.462–0.723), and W (kW ¼ 1.459–1.248), and
rameters of a ¼ 0.4901 nm and c ¼ 0.7840 nm, c/a ¼ 1.60, which is has no obvious effect on the segregation behavior of other elements. And
consistent with the crystal structure of the MgZn2 type, and TEM-EDS when the addition of 0.01 wt% C promotes the segregation of Nb (kNb ¼
analysis shows that it is rich in Mo, Nb, and Cr elements, correspond- 0.499–0.378), Ti (kTi ¼ 0.723–0.544), and W (kW ¼ 1.248–1.396). Such
ing to Laves phase as found in Ref. [17]. The SAED pattern shows a results indicate that when the carbon content is 0.04 wt%, the degree of
face-centered cubic crystal structure of the blocky phase(Fig. 3b) with a element segregation is higher than that of the other two alloys.
parameter of a0.424 nm, TEM-EDS analysis shows that they are rich in Segregation of alloying elements is accompanied by complex

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Fig. 2. SEM images showing dendritic structures of different carbon weights.

(a, d) C-0.01; (b, e) C-0.04; and (c, f) C-0.08.

carbides begin to be formed in alloy C-0.04. Additionally, with the

Table 3
further increase of C from 0.04 to 0.08 wt%, MC carbides increase
Secondary dendritic arm spacing of different carbon addition alloys(wt. %).
significantly. But the volume fraction of the (γþγ0 ) eutectic(7.77–0.06%),
C-0.1 C-0.4 C-0.8 Laves phase(3.09–0.27%) and η(2.81–0%)phase reduces sharply. The
SDAS(μm) 61.7  2.1 57.4  1.4 51.8  1.1 change in the precipitation phase is similar to the element segregation in
Fig. 5a. In summary, the addition of 0.04 wt% carbon promotes the
formation of the Laves phase, the (γþγ0 ) eutectic and the η phase, while
precipitates. Fig. 5b shows the volume fraction of the precipitated phase the addition of 0.08 wt% carbon inhibits the production of these
according to SEM image analysis. It can be seen that with the increase of precipitated phases. This can be attributed to the high production of the
carbon content from 0.01 to 0.04 wt%, the volume fraction of the (γþγ0 ) (Nb, Ti)C carbides, which depletes the constituent elements of the
eutectic(5.01–7.77%) and Laves phase(2.03–3.09%) increase greatly, eutectic (γþγ0 )-Ni3AlTi and η-Ni3Nb phases, resulting in a reduction of
and the volume fraction of η phase(2.44–2.81%) increases, too. The the precipitated phase content.
solubility of C in the C superalloys is very limited [31] until the MC

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Table 4
Chemical composition of precipitates in alloy GH4151 measured by EPMA (wt.%).
ID phase C Al Ti Cr Co Ni Nb Mo W
0
Pase A (γþγ ) 3.91 4.28 5.67 2.47 9.33 55.97 4.60 1.35 2.20
Pase B η 5.07 2.09 5.52 2.76 10.37 51.19 9.66 3.01 2.50
Pase C Laves 5.10 0.19 0.80 10.05 13.96 20.84 13.51 17.62 4.07
Pase D MC 14.30 0.11 17.09 0.34 0.38 1.31 59.64 6.54 0.81

Fig. 3. TEM images and the corresponding selected area diffraction patterns of the precipitates in the as-cast C-0.04 alloy: (a) Laves phase; (b) MC-carbide; (c) eutectic
(γ þγ0 ); (d) γ0 phase.

3.3. Phase transformation temperatures low-melting brittle phases, such as the Laves phase and the γþγ0 eutectic
phase precipitated in the interdendritic region.
Fig. 6 shows the DSC temperature rise curves of GH4151 alloy with a In addition, the carbon content increases do not have much influence
carbon content of 0.01 wt% C, 0.04 wt% C and 0.08 wt% C, which can be on the γ0 phase but have a significant impact on MC carbide. In the low-
used to determine phase transformation temperatures. There are three carbon C-0.01 alloy, the carbon is almost entirely solid-soluble in the
exothermic peaks in the heating curve. Due to the small volume fraction matrix, and the MC carbide is less abundant. Moreover, no heat ab-
of Laves, (γ þ γ0 ) and η phase the influence of its melting on heat flow is sorption peak of the MC carbide was detected in the DSC curve of C-
not enough to be reflected in the DSC curve. The DSC temperature rise 0.01(Fig. 6a). Then, with the increase of carbon content from 0.04 to
curves are divided into three types: start temperature, peak temperature, 0.08 wt%, the dissolution temperature of the MC carbide from 1291
C to
and end temperature. The results are shown in Table 5. As can be seen, 1297
C.
compared with the alloy C-0.01(Fig. 6a), the addition of 0.04 wt % To verify the test results of DSC curves and the effect of the precipi-
C(Fig. 6b) reduces the solidus temperature (TS) from 1267
C to 1255
C, tation phase on the initial melting temperature of the alloy, a water
the liquidus temperature (TL) from 1354
C to 1351
C, and the solidi- quenching test was carried out at 1290
C for 15 min. It can be seen from
fication temperature range(TL-TS) of alloy C-0.04 (96
C) is wider than the water quenching results in Fig. 7. When the temperature rises to
that of alloy C-0.01 (87
C). But reduces the solidification temperature 1290
C, melt pools appear between the interdendritic of C-0.01 and C-
range of alloy C-0.08 to 83
C(Fig. 6c). It is noted that the wider solidi- 0.04 alloys. In contrast, only a few melt pool patterns appeared in the C-
fication range of the alloy C-0.04 has a higher fusion enthalpy(817.0), 0.08 alloy. The total amount of low melting point precipitated phases in
compared with the fusion enthalpy of alloy C-0.01(506.1) and C- C-0.01 and C-0.04 alloys are more than that in C-0.08, which is consistent
0.08(520.0). It is consistent with the statistical results of the volume with the results of the statistics in Fig. 5b. Notably, a small amount of
fraction of precipitated shown in Fig. 5b. That is, in C-0.04 alloys more unfused MC carbide is observed in alloy C-0.04, while the melt pool

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Fig. 4. EBSD diagrams and pole figures of GH4151 alloys with different carbon content: (a, a') C-0.01; (b, b') C-0.04; (c, c') C-0.08.

Fig. 5. (a) Average distribution coefficient k [32], (b)Effect of carbon on precipitated phase and secondary dendrite spacing.

morphology shows a discontinuous distribution of broken points. This MC carbides gradually rise with the increase in carbon content. The inset
can be interpreted as the separation of MC relative to the existing liquid of Fig. 8b shows the variation curves of precipitation amount of MC
pool. It can be inferred that the melt pool formation will be unfavorable carbide and M23C6 phase with temperature, MC carbides may degrade
with the high carbon content. Conversely, during the cooling of the alloy, between 715 and 759
C due to MCþγ→ M23C6þγ0 reaction, and M23C6
the MC carbide has the potential to become a nucleation mass for the carbides precipitate at 715
C [33]. From the figure, it can be seen that
dendrites, which will promote the solidification of dendrites [31]. the carbide increases with increasing carbon content, M23C6 satisfies the
relation (1) y ¼ 0.23x and MC satisfies the relation (2) y ¼ 0.1x. With the
increase of carbon C from 0.01 to 0.04 wt%, the precipitation tempera-
3.4. Thermodynamic calculation
ture of MC carbide increased from 1237
C to 1305
C, and to 1329
C in
alloy C-0.08. Therefore, the precipitation temperature of carbide can be
Taking the standard composition and temperature parameters of
increased with the increase in carbon content.
GH4151 alloy as the input conditions of Thermo-calc software by equi-
librium calculation model, the change law of precipitates was obtained
by changing the carbon content in the alloy. From the calculation results 3.5. Tensile properties
in Fig. 8a, we can know that the change of carbon content has little effect
on the precipitation temperature and precipitation amount of γ0 phase in Fig. 9a shows the tensile curves of the as-cast GH4151 alloys with
the alloy, and has no effect on the solidus and liquidus temperature of the different carbon contents at 1100
C. The mechanical properties of the
alloy. This is because our calculations are performed by an equilibrium alloy are summarized in Fig. 9b. It can be seen that when the addition of
calculation model. This model assumes that solutes can be perfectly carbon from 0.01 wt% to 0.04 wt%, the ultimate tensile strength
mixed in the liquid phase and that there is solute back diffusion in the (130.7–442.3 MPa) and fracture elongation(0.73–11.26%) of the alloy
solid phase. The addition of carbon does not lead to an increase in the increase greatly, and the hardness (405-420 HV) of the alloy increases,
amount of segregation in the liquid phase, hence, the solidus tempera- too. Additionally, with the further increase of C from 0.04 to 0.08 wt%
tures calculated by Thermo-calc do not have much effect by carbon reduces the ultimate tensile strength (442.3–248.2 MPa) and fracture
addition. But the precipitation temperature and precipitation amount of elongation (11.26–1.90%) of the alloy, but the hardness of the alloy

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Fig. 6. The DSC heating curves of different carbon addition in the alloy: (a) C-0.01; (b) C-0.04; (c) C-0.08.

Table 5
Summary of solidification reaction temperatures (
C) in the DSC curves in Fig. 6.
Alloys P1 P2 P3 onset P3 P3 end △TL-S Fusion enthalpy

C-0.01 1145 – 1274 1336 1354 80 506.1

C-0.04 1148 1291 1255 1334 1351 96 817.0
C-0.08 1145 1297 1269 1335 1352 83 520.0

Fig. 7. Interdendritic structures of the alloys soaked at 1290
C for 15 min, then quenched in water: (a) C-0.01; (b)C-0.04; (c)C-0.08.

increases from 420HV to 435HV. In summary, the high-temperature 3.6. Fracture morphology
mechanical properties of C-0.04 alloy are better than C-0.01 and C-
0.08 alloy. In addition, all the alloys studied show high yield strength and The fracture surface characteristics of the alloys with different carbon
low fracture plasticity, which is different from the mechanical properties contents are shown in Fig. 10. It is clear that carbon significantly affects
of most austenitic stainless steels. This is because the stacking fault en- the fracture behavior of conventional cast alloys. The C-0.01 alloy mainly
ergy (SFE) of the GH4151 superalloy (172.6 mJ/m2) is much higher than exhibits fracture along the crystal. Fishbone patterns and intergranular
that of austenitic stainless steel(＜45 mJ/m2) [34]. In superalloys with fractures of long grains of non-micro-pit type were observed on the
high layer dislocation energy and weak interfacial stability, dislocations fracture surface (Fig. 10a, d). However, plastic deformation occurs in the
hardly separate and are not susceptible to deformation twinning, C-0.04 alloy. Inclined shear lip morphology zones and uneven fibrous
resulting in poor plasticity. morphology zones were observed at the edges of the microfracture
specimens. Typical laminar flow patterns were formed on the

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Fig. 8. (a) Relationship between precipitation amount and temperature of different carbon addition, (b) view a larger version.

Fig. 9. (a)Engineering stress-strain curves of alloys with different carbon content of the GH4151 alloys at 1100
C, (b) Effect of carbon on mechanical properties of
GH4151 alloy.

microfracture, mainly manifesting as complex quasi-cleavage and ductile temperature range are crucial to determine the shrinkage strain of metal
features (Fig. 10b, e). While for the C-0.08 alloy, obvious secondary materials during solidification. With the addition of carbon to the alloy,
cracks and casting dendrites can be observed (Fig. 10c, f), indicating that the alloy's average grain size and solidification temperature range are
the fracture mechanism of the C-0.08 alloy is consistent with typical simultaneously changed. With an increase in the carbon content from
dissociative fracture characteristics. In a word, the transition from the 0.01 to 0.04 and 0.08 wt%, the grain sizes decrease from 61.7 to 57.4 and
complete intergranular fracture in the C-0.01 alloy and C-0.08 alloy to 51.8 μm, respectively, as shown in Fig. 2a-c. A similar phenomenon has
mixed failure in alloy C-0.04 implies a significant enhancement of GB been reported in the Xu et al. literature [37]. With an increase in carbon
strength with appropriate C addition. content from 0.009 to, 0.017, 0.040, and 0.092 wt%, the PDAS from 60.9
In addition, the longitudinal cross-sections of the tensile fracture to 57.5, 48.8, and 31.3 μm.
samples were observed using SEM, as shown in Fig. 10(g–i). It can be When a small amount of carbon is added to the alloy, the carbon can
seen that cracks are generated in MC carbides, γþγ0 , and Laves phases. solid-solve into the matrix. The solid solution of carbon in the γ matrix
The relatively large size and higher stiffness of the γþγ0 eutectic structure decreases with the increase of carbon content. The remaining carbon is
make it difficult for dislocations to shear, resulting in stress concentration easily enriched at the front of the solid-liquid interface during solidifi-
along their interfaces [35]. Moreover, since most MC carbides and γþγ0 cation. With the increase of carbon concentration in the solid-liquid
eutectic structures are distributed in the inter-dendritic regions, tensile interface the primary carbides were generated, causing constitutional
cracks extend along these areas, resulting in dendritic features on the supercooling. Therefore, the nucleation and growth of secondary den-
fracture surface, as seen in Fig. 10(a–c). On the other hand, due to the drites arm spacing will be promoted [38]. In addition, the crystallization
different linear shrinkage coefficients of carbides and γþγ0 eutectic with process can be explained by Flemings’ dendrite growth mathematical
the matrix and insufficient liquid-phase compensation causing loose model, see Eq. (3) [39].
defects [9], see the inset map in Fig. 10h, cracks easily form along the
interface of MC carbides and γþγ0 eutectic structures, leading to fracture  13tc13
σ DL TL
under stress. d (3)
ρs HCl ð1  KÞmL

4. Discussion Among them, the d, tc, σ , DL, TL, ρs, H, and mL are the dendrite spacing,
dendrite coarsening time, solid-liquid interface energy, element diffusion
Carbon addition significantly affects the microstructure and me- coefficient in the liquid phase, liquidus temperature, solid density,
chanical properties of the GH4151 superalloy. This section discusses the melting latent heat, and liquidus slope, respectively. In the C-0.04 alloy,
effects of carbon addition on dendrite growth, microsegregation, the formation of the MC carbide prevents the solute elements in the liquid
precipitated phase, and tensile properties. phase from diffusing into the solid phase, thus decreasing the solute
partition coefficient K. Increasing the partition coefficient (1-K) also
4.1. Effect of carbon content on dendrite growth raises the solute concentration Cl in the dendritic arm. Therefore, the
secondary dendrites arm spacing(SDAS) will decrease according to Eq.
According to the strain theory [36], the grain size and solidification (3).

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Fig. 10. Fracture morphology and the longitudinal section of the as-cast GH4151 superalloys: (a, d) C-0.01; (b, e) C-0.04; (c, f) C-0.08.

4.2. Effect of carbon content on microsegregation fraction of Nb elements are used to generate NbC due to the low carbon
content, and most of the Nb elements are segregated into the mushy zone.
Several researchers have discussed reducing segregation by adding The segregation of Nb elements would offset the density difference and
carbon gradually [31]. However, this paper found that the C-0.04 alloy suppress the thermal solutal convection due to the high density of Nb. In
had the most severe deviations, followed by C-0.01, and the C-0.08 alloy addition, the NbC carbide also retards the local fluid flow. So the
had minor variations. Thermal solutal convection may be the significant segregation degree of Nb in C-0.04 is more significant than in C-0.01 and
factor affecting the segregation of solution elements. During solidifica- C-0.08. The mechanism of carbide influence on elemental segregation is
tion, the segregation of solution elements, such as W, Cr which segregate shown in Fig. 11.
to the dendrite core, and elements such as Mo, Nb, and Ti are rejected to Meanwhile, HU et al. [37] found that rhenium, tungsten, tantalum,
the interdendritic region, making the interdendritic liquid have an and aluminum segregation was more severe, with a carbon addition of
average density lower than that of the liquid above it. This density dif- 0.04%. Then the segregation degree decreases when the content of car-
ference caused by the segregation of solute elements results in the bon reaches 0.085%. This result is consistent with the study of this paper.
lower-density liquid at the bottom of the interdendritic region flowing up This is because of the addition of niobium and tantalum elements in this
to the top of the mushy zone, which may contribute to the homogeni- paper and HU's study, respectively. The tantalum and niobium elements
zation of solution elements. belong to the same VB group, which are segregated into the interden-
In this work, the content of Al þ Ti þ Nb exceeds 10 wt%, with the dritic during the solidification and tend to form the MC carbide to change
element Nb reaching 3.4 wt%. In the C-0.08 alloy, a large amount of Nb the thermal solute convection of the alloy.
elements in the mushy region are depleted to form the MC carbide, where
the consumption of Nb elements is greater than that of Ti elements. The
precipitation of Nb-rich carbides aggravates density inversion since it 4.3. Effect of carbon content on the precipitated phase
would delete Nb in the liquid. With the continuous depletion of Nb ele-
ments, the liquid density in the mushy zone decreases, allowing the 4.3.1. Carbides
thermal solute convection to be promoted. Therefore, more vigorous In the C-0.01 alloy, the precipitation amount of the MC phase is
thermal solutal convection would decrease the segregation in C-0.08 minimal. This is because carbon is mainly dissolved into the matrix by
compared to that in C-0.04. In contrast, in the C-0.04 alloy, only a tiny interstitial atoms. In the C-0.01 alloy, the content of Nb and Ti in the
liquid phase is high, but the carbon content is negligible. It is difficult to

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Fig. 11. Model diagram of solidification segregation of alloys with different C content.

reach the critical concentration of (Nb, Ti)C precipitation, making it phase. The precipitation of the Laves phase is usually located on both
difficult for the carbide phase to precipitate. However, in the high-carbon sides of the η phase and in front of the (γþγ0 ) eutectic phase. This phe-
C-0.08 alloy, the carbon enrichment is more accessible than in C-0.01 and nomenon is evident in the C-0.01 and C-0.04 alloys, see Fig. 2d and e. In
C-0.04 alloys. Hence, the carbides would be precipitated at an earlier the C-0.08 alloy, the Nb element in the remaining liquid is heavily
stage with a smaller solid fraction. This result can be reflected in the DSC consumed by the carbide. The precipitation of eutectic and η phases is
curves see Fig. 6. suppressed simultaneously, and the enrichment of Cr, Co, Mo, and Nb
In addition, the present work observed no morphological shift from elements is complex, reducing the Laves phase. The Laves phase pre-
massive to elongated strips of the carbide phase with increasing carbon. cipitates in small quantities, and the morphology is mainly fine and
It can be found in Table 5 that the carbide dissolving temperature is lumpy [45].
measured to be 55
C below the liquidus temperature in C-0.08. The solid
fraction would be 63%, the onset of thermal solutal convection is 4.4. Effect of carbon content on mechanical properties
confined within the mushy zone, and carbide growth is inhibited.
Moreover, based on the minimum surface energy the equilibrium The mechanical properties of GH4151 casting alloy with different
morphology of MC carbides is the octahedron or blocky [40,41]. carbon contents are shown in Fig. 10. Interestingly, when the carbon
addition is 0.04 wt%, the total precipitated phase is more significant than
4.3.2. (γþγ 0 ) phase 0.01 wt%, but the high-temperature mechanical properties of the C-0.04
It is well known that the generation of precipitated phases is influ- alloy are better than those of the C-0.01 and C-0.08 alloys. It has been
enced by elemental segregation. The results in Fig. 5b show that by reported in the literature that the solid solution effect of carbon in alloys
adding 0.01, 0.04, and 0.08 wt% carbon, the eutectic phase increased is limited [46]. When the carbon content increases to 0.04 wt%, most of
from 5.01% to 7.77% and reduced to 0.06%. This is because Nb is the the carbon is solid solution reinforced into the matrix. Part of the carbon
main element composing the MC carbides and the eutectic forming ele- forms a delicate MC carbide to strengthen the grain boundaries and
ments are mainly Ti and Al. In the C-0.04 alloy, the thermal solute con- enhance the mechanical properties of the alloy. With the further increase
vection is suppressed due to the segregation of Nb elements. As a result, of carbon to 0.08 wt%, a small part of carbon is dissolved into the matrix.
many Nb and Ti elements are segregated into the interdendritic, forming Most of the carbon forms the MC carbide in the dendrite stem, which
eutectic and Laves phases. But when the carbon content increases to 0.08 becomes the crack's origin and worsens the alloy's mechanical properties.
wt%, the carbides consume most of the Nb and little Ti elements. Thus As described in Ref. [12], a small amount of carbon addition is consid-
the thermal solute convection is promoted, and the elemental segregation ered beneficial to improve the mechanical properties of the alloy. The
is reduced. In this case, Ti concentration in the liquid pools could not be literature has reported that with the rise of carbide content in the alloy,
accumulated to the critical value for the precipitation of eutectic (γ þ γ0 ) more carbides will be precipitated at the grain boundaries, and their
and hence reduce its size and volume fraction [42]. tendency to coarsen into films is more prominent, which will directly
lead to the reduction of alloy toughness.
4.3.3. η phase Moreover, the literature has proposed that controlling the carbide
Table 4 shows that Mo, Cr, Co, and Nb elements are enriched in the number density is an alternative way to control and reduce thermal
Laves phase, and Ti and Al are enriched in the η-Ni3(Ti, Nb) and (γþγ0 ) cracking during solidification. This is because MC carbides contain about
eutectic. Moreover, as can be seen in Fig. 5b, the area fraction of the 5 at.% of H and O, which are the main elements for forming pores during
eutectic phase is always higer than that of the η phase. It is generally solidification [47]. Moreover, as seen in Fig. 12, the reduction of solid-
known that the increase in Ti/Al ratio favors η formation, and the ification defects in C-0.04 alloy makes the mechanical properties of
decrease in Ti/Al ratio is unfavorable for η formation [43,44]. The Ti C-0.04 alloys superior to those of C-0.01 and C-0.08 alloys [48].
content and critical subcooling required for forming the eutectic phase
are more accessible to achieve than for the η phase. The formation of the 5. Conclusion
eutectic phase consumes the Ti in the remaining liquid, making it
impossible to precipitate the η phase [42]. The volume fraction of the In this paper, the effects of interstitial carbon atoms on the micro-
eutectic degree is increased by 2.77%, while the η phase is increased by structure, microsegregation, and properties of a new nickel base super-
only 0.37%. In the high-carbon C-0.08 alloy, no η phase was formed. alloy were studied. The following important conclusions can be drawn:

4.3.4. Laves phase 1) The solid solution effect of carbon in the alloy is limited, when the
Meanwhile, the precipitation process of the η phase and (γþγ0 ) contents of C reach their solubility limit, MC carbides form in the as-
eutectic stage rejects Cr, Co, Mo, and other elements into the remaining cast microstructure. With the moderate increase of carbon content the
liquid. It forms Laves phase with the Nb elements enriched in the liquid secondary dendrite spacing is refined and no morphological shift

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Fig. 12. Morphology of GH4151 alloy with different C content before and after homogenization
(a, d) C-0.01 wt% C; (b, e)C-0.04; (c, f)C-0.08.

from massive to elongated strips of the carbide with the carbon Acknowledgments
addition, but rises the precipitation temperature of the MC carbides is.
2) Due to the influence of the high density of the Nb element, the most The authors gratefully acknowledge financial support from the Na-
severe segregation is found in the C-0.04 alloy, which promotes the tional Science and Technology Major Project (J2019-VI-0006-0120), the
formation of many low-melting brittle phases (γþγ0 , Laves, and η National Key R&D Program of China (2021YFB3700402), and the Na-
phase), and expands the solidification temperature range. The solid- tional Natural Science Foundation of China (Grant No. 52074092,
ification ranges of C-0.01, C-0.04, and C-0.08 alloys are 87
C, 96
C, 52274330).
and 83
C, respectively.
3) The moderate increase of carbon content greatly decreases the so- References
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