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Investigation of Solidification and Segregation Characteristics of Cast Ni-Base

Superalloy K417G

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DOI: 10.1016/j.jmst.2016.11.009

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 Journal of Materials Science & Technology 34 (2018) 541–550

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Investigation of Solidification and Segregation Characteristics of Cast

Ni-Base Superalloy K417G
Li Gong, Bo Chen, Zhanhui Du, Mengshu Zhang, Ruichang Liu, Kui Liu
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: Differential scanning calorimetry (DSC) analysis, isothermal solidification experiment and Thermo-Calc
Received 19 August 2016 simulation were employed to investigate solidification characteristics of K417G Ni-base superalloy. Elec-
Received in revised form 6 October 2016 tron probe microanalysis (EPMA) was employed to analyze the segregation characteristics. Liquidus,
Accepted 31 October 2016
solidus and the formation temperatures of main phases were measured. In the process of solidification,
Available online 9 November 2016
the volume fraction of liquid dropped dramatically in the initial stage, while the dropping rate became
very low in the final stage due to severe segregation of positive segregation elements into the residual
Key words:
liquid. The solidification began with the formation of primary ␥. Then with solidification proceeding, Ti
K417G superalloy
Solidification characteristics
and Mo were enriched in the liquid interdendrite, which resulted in the precipitation of MC carbides in
Segregation the interdendrite. Al accumulated into liquid at the initial stage, but gathered to solid later due to the
Isothermal solidification precipitation of ␥/␥ eutectic at the intermediate stage of solidification. However, Co tended to segregate
Thermo-Calc simulation toward the solid phase. In the case of K417G alloy, combining DSC analysis and isothermal solidification
experiment is a good way to investigate the solidification characteristics. Thermo-Calc simulation can
serve as reference to investigate K417G alloy.
© 2017 Published by Elsevier Ltd on behalf of The editorial office of Journal of Materials Science &
Technology.

1. Introduction better performance for K417G alloy[12] . Actually, cracks forming

Nickel-base superalloys have been extensively studied on multi-
fields for 50 years and widely used for hot components of gas
turbine engines[1–3] . In100 Ni-base, superalloy has been widely
used in the aeroengine turbine casts due to its low density and
excellent mechanical properties. However, high content of Ti in
In100 alloy results in lots of cast porosities and ␴ phases[4,5] .
In order to reduce these detrimental phases, Chinese scien-
tists adjusted its compositions and casting parameters[6–8] . Then
through reducing the contents of Ti and Co, K417G superalloy was
developed.
Cast K417G superalloy, used as the aeroengine turbine blades,
has excellent yield and tensile strength and high-temperature
oxidation resistance at elevated temperature[9–11] . The common
process of manufacturing K417G consists of vacuum induction
melting (VIM) and casting into turbine blades. With increas-
ing the rotational speed of the engine, turbine blades need to
work at critical conditions of severer creep, higher temperature,
greater stress and fatigue for more than 70,000 h, which demands
∗ Corresponding author. Fax: +86 24 23906716;
E-mail address: bchen@imr.ac.cn (B. Chen).
in the blade always result in the failure of turbines during work-
ing. The crack is known as hot tearing, which is linked to the
solidification behavior[13,14] . Studies show that hot tearing gener-
ally occurs at the terminal stage of solidification, when the melt
is difficult to compensate for shrinkage[15] . Moreover, the cracks
always expand in the interdendrite, where there are numerous of
carbides, micro-porosities and ␥/␥ eutectics. Degenerated MC car-
bides would accelerate the expansion of microcracks[16] , and the
␥/␥ eutectic is a deleterious phase with lower strength typically
as the crack origin[17] . Therefore, detailed knowledge of solidifi-
cation nature is important for improving the cast properties and
controlling the hot tearing of K417G alloy.
In addition, segregation during solidification process con-
tributes to the formation of casting defects[18] , and hot tearing
susceptibility is significantly influenced by the contents of alloying
elements[14] . For superalloy In100, the strong segregation of Ti into
the liquid results in lots of micro-porosities[4,5] . Thus, decreased
contents of Ti and Co in K417G alloy have an effect on the solidifi-
cation behavior and the hot tearing formation.
However, until now, researches about K417G nickel-base super-
alloy mainly focus on microstructures and mechanical properties.
Further studies on the solidification and segregation behavior of

https://doi.org/10.1016/j.jmst.2016.11.009
1005-0302/© 2017 Published by Elsevier Ltd on behalf of The editorial office of Journal of Materials Science & Technology.
542 L. Gong et al. / Journal of Materials Science & Technology 34 (2018) 541–550
K417G alloy are still necessary for better controlling casting defects.
In this study, differential scanning calorimetry (DSC) analysis,
isothermal solidification experiment and Thermo-Calc simulation
were employed to investigate solidification behavior, including liq-
uidus, solidus, the formation temperatures of main phases and
solidification sequence. Electron probe microanalysis (EPMA) was
employed to analyze the segregation characteristics.
2. Experimental Procedures
2.1. Materials and DSC analysis
The master ingot of K417G superalloy used in this work was
prepared by vacuum induction melting (VIM) and the chemical
composition of K417G superalloy is listed in Table 1. The samples
from the master ingot were observed by optical microscopy (OM)
and scanning electron microscopy (SEM) to obtain major phases of
K417G alloy.
To estimate the transformation temperatures of main phases,
DSC tests were performed on the SETARAM SETSYS Evolution 18
testing apparatus. The thermocouples of DSC instrument were cal-
ibrated with high purity Au (99.9999%), Ag (99.99%) and Ru (99.99%)
with the heating rate of 10 ◦ C/min. The specimen used in the DSC
testing was cut from the master alloy and the mass was 32.68 mg.
All the experiments were conducted in a dynamic high-purity Ar
atmosphere with high-purity Al2 O3 crucibles to minimize the effect
of oxidation. The specimens were subjected to heating and cooling
cycles as follows:
Room temperature → heating at 30 ◦ C/min up to 1000 ◦ C →
isothermal holding at 1000 ◦ C for 10 min → heating at 10 ◦ C/min
up to 1450 ◦ C → isothermal holding at 1450 ◦ C for 10 min → cool-
ing at 10 ◦ C/min down to 1000 ◦ C → cooling at 30 ◦ C/min down to
room temperature.
The chosen cooling rate (10 ◦ C/min) typically coincides with
that in the industrial casting process. The experimental procedures,
parameters selection, and data calibration are all referred to gen-
eral principles of DSC testing[19,20] . According to general principles,
the solidus is obtained from the heating curve, and the liquidus is
obtained from the cooling curve[18–21] .
2.2. Isothermal solidification process and microstructure analysis
Specimens used in the isothermal solidification experiment
were cut from the master alloy with the size of ␾ 16 mm × 10 mm.
The samples were put into the alumina crucibles and covered with
the alumina powder to minimize the oxidation effectively. The
isothermal solidification process was shown in Fig. 1. The packaged
samples in the furnace were heated up to 1450 ◦ C and isothermally
held for 15 min to homogenize the melt, followed by cooling at
10 ◦ C/min down to different isothermal solidification temperatures
Fig. 1. Isothermal solidification process with different isothermal temperatures
ranging from 1360 ◦ C to 1220 ◦ C at the interval of 10 ◦ C.
ranging from 1360 ◦ C to 1220 ◦ C at the interval of 10 ◦ C for 10 min,
and then subsequently quenched into the salty water.
To determine the volume fraction of the residual liquid in the
isothermal solidification samples, the samples were etched with
the solution of 20 g CuSO4 + 100 mL HCl + 5 mL H2 SO4 + 100 mL H2 O.
Seven images with 100× magnification were randomly captured at
different areas of each sample by OM. The volume fraction of resid-
ual liquid was measured by Sisc IAS image analysis system, and the
average value was taken. The solidification microstructures with
different isothermal temperatures were analyzed by OM and SEM.
EPMA was employed to investigate the element concentration and
distribution on the un-etched samples with different isothermal
temperatures. The samples for transmission electron microscopy
(TEM) were prepared by jet-beam electro-polishing in a solution of
10% perchloric acid and 90% ethanol between −17 ◦ C and −23 ◦ C.
2.3. Thermo-Calc simulation
The Thermo-Calc software and TTNI8 database were employed
to calculate solidification sequence of K417G alloy. The chemical
composition input in this program is listed in Table 1. The simula-
tion was performed under equilibrium condition and the program
proceeded to step down every 10 ◦ C from 400 ◦ C to 1600 ◦ C. At each
temperature step, the program would determine the equilibrium
phase according to the lowest Gibb’s energy. For comparison, the
solidification sequence was also calculated according to the Scheil
model and TTNI8 database. The Scheil simulation was under the
non-equilibrium condition based on the correction of the segrega-
tion coefficient. The Scheil model proceeded to step down every
1 ◦ C until the complete solidification.
3. Results
3.1. Results of DSC analysis
The DSC curves of the K417G alloy during heating and cooling
process are presented in Fig. 2. Several transformation tempera-
tures of main phases were obtained. The solidus temperature was
1293 ◦ C obtained from the intersection of the extrapolated baseline
and the tangent of the maximum curve slop in the heating curve,
and the liquidus temperature was 1333 ◦ C obtained from the first
sharp inflection point in the cooling curve[18–21] .
From the heating curve, three major phase transformations
could be observed: (1) the dissolution of ␥ phases into the matrix;
(2) the dissolution of carbides; (3) the melting of the ␥ matrix.
From the cooling curve, four major phase transformations could
be observed: (1) the sharp peak corresponding to the formation of
the ␥ dendrite; (2) the precipitation of carbides; (3) the formation of
␥/␥ eutectics; (4) the precipitation of ␥ phases from the ␥ matrix.
As detailed listed in Table 2, the phase transformation tempera-
tures obtained from the cooling curve are lower than those from
the heating curve as a result of the superheating and supercooling
effects on the phase transformation.
3.2. Solidification process
The evolution of microstructures from the isothermal solidifica-
tion followed by quenching experiments is showed in Fig. 3, which
reveals the relationship between the isothermal temperature and
the volume fraction of liquid during the solidification process. From
Fig. 3, the volume fraction of the residual liquid dropped dramat-
ically in the initial stage of solidification, while the dropping rate
slowed down at the final stage.
The solidified (S) and liquid (L) regions could be distinguished
clearly by the coarse and extremely fine dendritic structures,
respectively. From Fig. 3(a and b), the sample remained fully liquid
 L. Gong et al. / Journal of Materials Science & Technology 34 (2018) 541–550 543

Fig. 2. DSC results for K417G alloy: (a) heating and (b) cooling processes.

Fig. 3. OM and corresponding volume fraction of the liquid phase from isothermal solidification experiments on K417G alloy revealing the microstructure evolution. Solid
(S) and liquid (L) phases are clearly shown on samples quenched at: (a) 1350 ◦ C; (b) 1340 ◦ C; (c) 1300 ◦ C; (d) 1290 ◦ C and (e) 1270 ◦ C.

at 1350 ◦ C, but the dendritic structure became coarser at 1340 ◦ C
and the volume fraction of the liquid phase dropped to 82.8%. The
results indicated that the liquidus temperature lay between 1340 ◦ C
and 1350 ◦ C, and it was closer to 1340 ◦ C. With decreasing the
isothermal temperature, the dendrites grew very fast. At 1330 ◦ C,
the volume fraction of the liquid was 33.8%. At 1300 ◦ C, the liquid
volume fraction was 22.8%, and the residual liquid was still contin-
uous in the interdendrite channel (shown in Fig. 3(c)). At 1290 ◦ C,
most of the alloy had solidified and the isolated liquid pools were
observed (Fig. 3(d)), which restricted the flow of liquid between two
phases. The volume fraction of isolated liquid pools has reduced to
6.5% at 1280 ◦ C and was only 3.2% at 1270 ◦ C. Therefore, the solidus
temperature can be considered as 1270 ◦ C. In conclusion, the
solidification process of the K417G alloy can be summarized into
four stages as follows: (1) the formation of the primary dendrite;
(2) the growth of the primary dendrite; (3) the un-continuous net-
work of the liquid and the precipitation of the second phase; (4) the
complete solidification of the remaining liquid in the interdendrite.
3.3. Microstructure analysis
As shown in Fig. 4, the as-cast K417G alloy has a typical den-
dritic morphology with ␥ matrix, ␥/␥ eutectic, a few carbides and
micro-porosities in the interdendrite regions and cubic ␥ rein-
forced precipitates with 571 nm in the magnified Fig. 4(b).
544 L. Gong et al. / Journal of Materials Science & Technology 34 (2018) 541–550

Fig. 4. As-cast microstructure (a) and the morphology (b) of ␥ of K417G alloy.

Fig. 5. Precipitation process of carbides from isothermal solidification experiment at different isothermal temperatures: (a) and (b)1340 ◦ C, (c) and (d) 1330 ◦ C, (e) and (f)
1320 ◦ C.

After etching with the solution of 20 g CuSO4 + 100 mL HCl + 5 mL
H2 SO4 + 100 mL H2 O, the samples with different isothermal tem-
peratures were analyzed by OM. As shown in Fig. 5, the carbides
began to precipitate in the sample quenched at 1330 ◦ C. Big blocky
phases can be clearly found at the dendrite, which meant that they
formed in the solid. The energy spectrum analysis demonstrated
that the carbides were significantly enriched in Mo and Ti (Fig. 6(c)).
It is well known that Mo and Ti are strong former of carbides. More-
over, as illustrated in Fig. 6, the blocky carbide was FCC crystal
structure with the lattice constant a of 0.430 nm, which fell inter-
mediately between that of MoC (0.4273 nm) and TiC (0.4327 nm),
so the carbides might be MC ((Ti, Mo)C) carbides.
In addition, there were lots of tiny rod-like and nodular phases
precipitating at the interdendrite, as shown in Fig. 5. According to
EPMA map in the sample quenched at 1320 ◦ C, C, Mo and Ti were
significantly enriched in these phases, and V slightly gathered in
them, as illustrated in Fig. 7. Meanwhile, Ni was depleted in these
phases. Therefore, these tiny rod-like and nodular phases might
be MC ((Ti, Mo)C) carbides. With the solidification proceeding, C,
Mo and Ti were rejected to the residual liquid. The concentra-
tion of these elements resulted in the precipitation of MC carbides
from liquid phase in the quenching process. These tiny MC car-
bides formed in the quenching process can be clearly distinguished
from the blocky MC carbides precipitated during the solidification
process.
For better distinguishing the ␥/␥ eutectic from the residual liq-
uid, the isothermal solidification samples were electrolyzed with
10% phosphoric acid. There were white phases precipitating around
the liquid when the isothermal temperature was equal to or lower
than 1300 ◦ C, as clearly shown in Fig. 8. From the SEM images
 L. Gong et al. / Journal of Materials Science & Technology 34 (2018) 541–550 545

Fig. 6. TEM characterization of MC carbide in the sample quenched at 1280 ◦ C: (a) the morphology of MC carbide; (b) selected-area diffraction corresponding (a); (c) EDS
spectrum corresponding (a).

Fig. 7. Qualitative elemental mapping images of Ni, Al, Ti, Mo, C, Cr, Co and V in the sample quenched at 1320 ◦ C.

(Fig. 9), the white phases showed lamella structure, which were
␥/␥ eutectics precipitating at the frontier of liquid. One EPMA map
in the sample quenched at 1300 ◦ C was chosen to analyze the distri-
bution of elements, and the color contrast represented the degree of
segregation. As illustrated in Fig. 10, Mo, C, Cr and V were depleted
in the ␥/␥ eutectic, but Al and Ni were significantly enriched in the
␥/␥ eutectic. Moreover, Mo, Cr and V were enriched in the residual
liquid pools, and Ni and Al were depleted in the liquid. Meanwhile,
the content of Ti in the ␥/␥ eutectic and liquid phase was higher
than that in the solid phase. The energy disperse spectroscopy (EDS)
spectrum showed that the average chemical composition of the
␥/␥ eutectic was 70.86% Ni, 7.87% Co, 3.69% Cr, 10.38% Ti, 5.93% Al,
546 L. Gong et al. / Journal of Materials Science & Technology 34 (2018) 541–550

Fig. 8. Precipitation process of ␥/␥ eutectic from isothermal solidification experiment at different isothermal temperatures: (a) 1310 ◦ C, (b) 1300 ◦ C, (c) 1290 ◦ C and (d)
1280 ◦ C.

Fig. 9. SEM images of ␥/␥ eutectic in the sample quenched at 1300 ◦ C: (a) ␥/␥ eutectic precipitating from the liquid phase; (b) the morphology of ␥/␥ eutectic at frontier
of liquid.

0.82% Mo and 0.24% C (wt%). It was obvious that the contents of
Cr and Mo in the ␥/␥ eutectic were much smaller than their aver-
age contents in the alloy, so Cr and Mo had been rejected into the
residual liquid[22] .
3.4. Microsegregation analysis in K417G alloy
tended to gather in the liquid phase. The k values of Cr and V were
fluctuating around 1, which meant that these elements did not
incline to segregate toward solid or liquid phase. It is noted that
the k value of Al increased with decreasing the isothermal temper-
ature, which meant that Al was enriched in the solid phase during
the terminal solidification stage.

Alloying elements have different solubilities in the solid and liq-
uid phases. Therefore, with the proceeding of solidification, alloying
elements redistribute into the solid and liquid phases, which
results in elementary microsegregation[23] . EPMA was applied to
quantitatively investigate the elementary microsegregation with
different isothermal solidification temperatures. The solute parti-
tion coefficients (k) at different isothermal temperatures are listed
in Table 3,
ki = Ci,s /Ci,l
where Ci,s and Ci,l are the average concentration of the element
i in the solid and liquid phases, respectively[1] . The value of k
less than 1 indicates that the elements segregate to the liquid
phase, while k greater than 1 indicates that the elements segregate
to the solid phase[24] . As clearly shown in Fig. 11, Co was nega-
tive segregation element, which tended to segregate toward the
solid phase. Ti and Mo were positive segregation elements, which
3.5. Thermo-Calc simulation of solidification
The solidification sequence of K417G superalloy calculated by
the Thermo-Calc simulation is presented in Fig. 12. From the equi-
librium phase diagram (Fig. 12(a)), the ␥ matrix began to solidify at
1345 ◦ C corresponding to the liquidus and the solidification ter-
minated at 1296 ◦ C when the liquid fraction was zero. The MC
carbide precipitated at 1340 ◦ C; the M3 B2 boride precipitated at
1152 ◦ C; the M23 C6 carbide precipitated at 999 ◦ C and ␴ phase pre-
(1)
cipitated at 837 ◦ C in the cooling process. The ␥ phase precipitated
at 1219 ◦ C after the solidification of the ␥ matrix. The intersec-
tions of the ␥ matrix and ␥ phase suggested that the ␥/␥ eutectic
would form during the solidification. Moreover, a small number of
␮ phases would precipitate at lower temperature. In addition, the
solidification sequence calculated by Scheil model, which takes the
segregation of the solute elements into consideration, is presented
in Fig. 12(b). The Scheil model predicted that the formation of the ␥
 L. Gong et al. / Journal of Materials Science & Technology 34 (2018) 541–550 547

Fig. 10. Qualitative elemental mapping images of Ni, Al, Ti, Mo, C, Cr, Co and V in the sample quenched at 1300 ◦ C.

matrix was at 1346 ◦ C, corresponding to the liquidus temperature,

and the solidus temperature was 1150 ◦ C when the solid fraction
was 1.0. The MC carbide precipitated at 1330 ◦ C when the solid frac-
tion was 48%. The MB2 boride precipitated at 1289 ◦ C when the solid
fraction was 88%. The M3 B2 boride precipitated at 1262 ◦ C when the
solid fraction was 96%. The ␥/␥ eutectic formed at 1213 ◦ C when
the solid fraction was 98% and ␴ phase formed at 1175 ◦ C when
the solid fraction was 99%. From the results, it can be concluded
that the ␥/␥ eutectic in K417G alloy was a non-equilibrium phase
which was caused by the segregation of the solute elements during
the solidification.

4. Discussion

4.1. Solidification characteristics

From the DSC analysis, isothermal solidification experiment

and Thermo-Calc simulation results, the liquidus, solidus and the
transformation temperatures of main phases are summarized in
Table 4. The liquidus obtained from the Thermo-Calc simulation
is similar to that from the isothermal solidification experiment,
but slightly higher than DSC result. The specimen used in the
DSC experiment is very small (32.68 mg), and the cooling pro-
cess is relatively rapid (with a rate of 10 ◦ C/min), which increase
the supercooling degree of the melt[17] . Therefore, the actual crys-
tallization temperature is low. Owing to the great supercooling
in the solidification process, the liquidus from the DSC experi-
ment is relatively low, so the liquidus of K417G alloy is 1345 ◦ C.
The solidus obtained from the Thermo-Calc equilibrium model is
Fig. 11. Solute partition coefficient (k) on the samples quenched at different isother-
mal temperatures.
similar to the DSC result, but higher than the result obtained from
isothermal solidification experiment. Actually, the liquid volume
fraction is 100% at 1350 ◦ C and 33.8% at 1330 ◦ C. In the initial stage
of the solidification, a considerable number of liquid has solidified
which indicates that the dendritic crystals grow up dramatically.
The intermediate solidification stage covers from 1330 ◦ C to 1290 ◦ C
and the transformation rate of the solidification becomes slow.
548 L. Gong et al. / Journal of Materials Science & Technology 34 (2018) 541–550
Fig. 12. Simulation results of K417G superalloy calculated by Thermo-Calc: (a) equilibrium phases and their weight fractions corresponding to different temperatures, (b)
solidification sequence calculated by Scheil model.
The final solidification stage is from 1290 ◦ C to 1240 ◦ C. In this
stage, the residual liquid could be long-term reserved due to ele-
ments segregation into the residual liquid. Therefore, solidus from
the isothermal solidification experiment is low because of severe
segregation in the final solidification stage. In the Thermo-Calc
equilibrium model, the calculation is conducted under equilibrium
condition, which underestimates the segregation degree, so there
are no positive segregation elements gathering into the residual
liquid in the last stage of solidification. In the DSC experiment,
the solidus is obtained from the heating curve, so it is not affected
by elements segregation. Therefore, the solidus obtained from the
Thermo-Calc equilibrium model agrees with the DSC result, and it
is higher than the isothermal solidification result. In the industrial
casting process, the element segregation is inevitable, so it is more
reasonable to select 1270 ◦ C as the solidus of K417G alloy. Gener-
ally, when the solidification interval of alloys is wide, the feeding of
melt is more difficult in the last stage of solidification. Thus, the den-
dritic network is submitted to shear, and the hot tearing is easier to
form[25] .
The precipitation temperatures of main phases obtained from
the DSC experiment show many similarities to those measured by
the isothermal solidification experiment. In the DSC experiment,
the supercooling degree is great in the solidification process, so pre-
cipitation temperatures of main phases are lower than those from
the isothermal solidification experiment. However, the main phase
precipitation temperatures obtained from the Thermo-Calc simu-
lation show many differences from those measured by isothermal
solidification experiment. In the Thermo-Calc equilibrium model,
the calculation is conducted under ideal conditions, so the phase
transition temperatures are unreliable. Moreover, certain phases
(M3 B2 , ␮ phase and ␣-Cr) predicted by the Thermo-Calc simulation
are not found in K417G alloy. Indeed, when the content of boron is
greater than 0.8 wt%, the boride would precipitate from the liquid
in the reaction of L → ␥ + M3 B2 in the final stage of solidification[26] .
The content of boron is 0.023 wt% used in this work, so boride
precipitates are not found in solidification samples. Because the
Scheil model takes segregation of alloy elements into consideration
when calculating, the liquidus and MC carbide formation tempera-
ture match very well with the results from isothermal solidification
experiment. The Scheil model cannot simulate back diffusion into
the solid phase, so it would overestimate the segregation degree
of alloying elements in the residual liquid[27] . This is the reason
why the temperature range for MC carbide formation based on the
Scheil model is very wide (from 1330 ◦ C to 1289 ◦ C). In addition, at
the final stage of solidification, elements segregation in the residual
liquid will be more serious. It would contribute to the precipitation
of many phases (MB2 and M3 B2 ) and slow down the solidification
of residual liquid, which results in an extreme low solidus
(1150 ◦ C).
Therefore, liquidus predicted by the Thermo-Calc equilibrium
model and Scheil model is accurate, and solidus obtained from
Thermo-Calc equilibrium model and the precipitation temperature
of MC carbide based on Scheil model can serve as effective refer-
ences. The phase transition temperatures are not well predicted
by Thermo-Calc simulations. Combining the DSC results with the
analysis of isothermal solidification experiment is a good way to
predict the solidification behavior of K417G superalloy.
4.2. Segregation characteristics
From the previous EPMA results in Table 3 and Fig. 11, Ti and
Mo tend to segregate into the liquid, which means that these ele-
ments are enriched in the interdendritic region. The smaller the
k value less than 1 is, the stronger degree of segregation to the
interdendritic liquid is[15] . In the quenching process, the concen-
trations of Mo and Ti in the liquid phase will result in tiny nod-like
MC carbides precipitating in the liquid phase (Fig. 7). With the
solidification proceeding, MC carbides would form in the inter-
dendrite because of the concentrations of Mo and Ti in the liquid
phase.
From Fig. 11, the segregation behavior of Al is special. Its k
value is less than 1 when the quenching temperature is above
1300 ◦ C, but greater than 1 when it is equal to or below 1300 ◦ C.
Therefore, Al accumulates to the liquid in the initial stage of solid-
ification, but it gathers into the solid in the intermediate and last
stage of solidification. As shown in Fig. 13, the white line repre-
sents the position of line-scanning, and the curves with different
colors represent the content of different elements. The content
of Al is very low in the liquid phase, but it gathers in the ␥/␥
eutectic. In the process of solidification, the ␥/␥ eutectics precip-
itate from the liquid when the temperature drops to 1300 ◦ C. Al
is enriched in the ␥/␥ eutectic, which results in the decrease of
Al content in the residual liquid. The precipitation of ␥/␥ eutec-
tic gives good explanation to the special segregation behavior of Al
at different isothermal temperatures. Meanwhile, Mo, C and Cr are
significantly enriched in the residual liquid, but depleted in the ␥/␥
eutectic.
On the contrary, the k value of Co is greater than 1, so Co tends
to be depleted in the residual liquid, which means that Co would
segregate to dendrite cores. As shown in Fig. 13, the content of Co
is obviously lower in the ␥/␥ eutectic and liquid than that in the
matrix. With solidification proceeding, Ti and Mo constantly gather
into the residual liquid, which results in a very slow solidification
rate in the last stage of solidification.
 L. Gong et al. / Journal of Materials Science & Technology 34 (2018) 541–550
Fig. 13. Line-scanning images of Cr, Al, V, C, Co, Mo and Ti in the sample quenched at 1300 ◦ C.
4.3. Solidification sequence
The solidification sequence of K417G alloy has been identified
as follows:
(1) L → ␥. With the increase of undercooling, the nucleation and
growth of ␥ phase have been observed. Below the liquidus of
1345 ◦ C, ␥ dendrite grows dramatically. The negative segrega-
tion elements, such as Co, tend to segregate to the ␥ solid, while
the positive segregation elements, such as Al, Ti and Mo, tend
to accumulate to the liquid and then they are reserved into the
interdendrite[18] . With the increase of cooling rate, the segrega-
tion will be more severe[26] . Because some positive segregation
elements are enriched into the residual liquid, non-equilibrium
phase will precipitate from the liquid.
(2) L → ␥ + MC. With the solidification proceeding, the positive
segregation elements Ti and Mo accumulate into the residual
liquid, which promotes nucleation of MC ((Ti, Mo)C) carbides in
the interdendritic region[28] .
(3) L → ␥ + ␥ . When Ti and Al sufficiently accumulate into the resid-
ual liquid, the ␥/␥ eutectic will precipitate at the interdendritic
regions at the intermediate stage of solidification. As shown in
Fig. 10, Al and Ti are significantly enriched in the ␥/␥ eutectic,
so the content of Al in the residual liquid decreases due to the
formation of ␥/␥ eutectic at 1300 ◦ C. It is a reasonable expla-
nation to special segregation behavior of Al, which is clearly
shown in Fig. 11.
(4) ␥ → ␥ . As the temperature decreases, Ni, Al and Ti are super-
saturated in the ␥ matrix, then the ␥ precipitate will nucleate
and grow up from the ␥ matrix through the diffusion of atoms.
The solidification sequence of K417G superalloy can be summa-
rized as follows: (1) nucleation and growth of primary ␥ phase (L
→ ␥ at 1345 ◦ C); (2) MC carbides precipitate from the interden-
dritic liquid (L → ␥ + MC at 1330 ◦ C), where M mainly represents
Mo and Ti; (3) non-equilibrium ␥/␥ eutectic reaction (L → ␥ + ␥ at
1300 ◦ C); (4) the ␥ phases precipitate from the supersaturation ␥
matrix (␥ → ␥ at 1215 ◦ C).
5. Conclusions
Through DSC analysis, isothermal solidification experiment and
Thermo-Calc simulation, the solidification process and segregation
behavior of K417G alloy have been obtained as follows:
1. The liquidus and formation temperatures of main phases pre-
dicted by DSC analysis are slightly lower than those from the
549
isothermal solidification experiment, while the solidus is higher
than that from the isothermal solidification experiment. The
results from the two methods show many similarities, so com-
bining DSC analysis and isothermal solidification experiment is
a good way to investigate the solidification characteristics of
K417G superalloy.
2. Thermo-Calc simulation can accurately predict liquidus. How-
ever, the Thermo-Calc equilibrium simulation is conducted
under equilibrium conditions, so solidus based on it is higher
than that obtained from isothermal solidification experiment.
Due to overestimation of the element segregation into the
residual liquid, solidus based on Scheil model is extremely
low. Meanwhile, the phase transition temperatures predicted
by them are unreliable. Therefore, the liquid and solidus from
Thermo-Calc equilibrium model and the MC carbide precipita-
tion temperature from Scheil model can serve as references to
investigate K417G alloy.
3. With the solidification proceeding, Ti and Mo accumulate into
the residual liquid, which promotes the nucleation and growth
of MC carbides at the initial stage of solidification. Co tends to
segregate to the solid. Al accumulates to the liquid at the initial
time, but gathers into the solid later due to the precipitation of
␥/␥ eutectics at the intermediate stage of solidification.
4. The liquidus of K417G alloy is 1345 ◦ C, and the solidus is
1270 ◦ C. In the last stage of solidification, because of alloying
elements gathering into the residual liquid, the solidus will be
low.
5. The solidification sequence of K417G superalloy can be identified
as follows: L → ␥ at 1345 ◦ C; L → ␥ + MC at 1330 ◦ C; L → ␥ + ␥ at
1300 ◦ C; ␥ → ␥ at 1215 ◦ C.
Acknowledgment
The authors would like to thank Miss Shuang Qu for her help in
DSC measurements.
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