Slip Casting
Slip Casting
a r t i c l e i n f o a b s t r a c t
Article history: The effects of different solidification rates after pouring on the microstructures, microsegregation and
Received 25 April 2016 mechanical properties of cast superalloy K417G were investigated. Scheil-model was applied to calculate
Received in revised form 16 June 2016 the temperature range of solidification. The casting mould with different casting runners was designed
Accepted 27 February 2017
to obtain three different cooling rates. The microstructures were observed and the microsegregation
Available online 30 March 2017
was investigated. Also, high temperature tensile test was performed at 900 ◦ C and stress rupture test
was performed at 950 ◦ C with the stress of 235 MPa. The results showed that the secondary dendrite arm
Keywords:
spacing, microsegregation, the size and volume fraction of phase and the size of / eutectic increased
Ni-based cast superalloy
Cooling rate
with decreasing cooling rate, but the volume fraction of / eutectic decreased. In the cooling rate range
Microstructure of 1.42 ◦ C s−1 –0.84 ◦ C s−1 , the cast micro-porosities and carbides varied little, while the volume fraction
Microsegregation and size of phase and / eutectic played a decisive role on mechanical properties. The specimen with
Mechanical property the slowest cooling rate of 0.84 ◦ C s−1 showed the best comprehensive mechanical properties.
© 2017 Published by Elsevier Ltd on behalf of The editorial office of Journal of Materials Science &
Technology.
1. Introduction elements and the growth of main phases. So the cooling rate has a
significant effect on the mechanical properties for casting superal-
Nickel-based superalloys are widely used in turbine compo- loy. Therefore, a complete description of the effect of cooling rate
nents of aircraft engines because of its excellent mechanical on K417G alloy is required.
properties under critical and severe service conditions [1–4]. Cast Most investigations focused on the effect of cooling rate during
superalloy K417G is used for the aeroengine turbine blade, which solidification process give a wide range of solidification cooling rate
is one of the most important parts of the engine working under [8,10–13]. However, the differences of cooling rate caused by dif-
the condition of high temperature up to 1100 ◦ C. The turbine blade ferent thickness in the turbine blade are small. So there is no critical
needs to sustain the centrifugal force generated by its own weight, conclusion which is closely linked to industrial production. Mean-
aerodynamic force generated by air and gas, thermal stress and while, most of these investigations are concerned on the effect of
vibration stress at the same time [5]. Therefore, K417G superalloy cooling rate on microsegregation and microstructure, but few are
requires excellent yield and tensile strength, high hot-corrosion concerned on mechanical properties.
and high-temperature oxidation resistance, enough ductility, ade- In this work, the casting mould with three different casting run-
quate endurance and creep strength, and good microstructure ners was designed to simulate different cooling rates in different
stability at high temperature [6,7]. parts of the turbine blade. All of the runners share a same runner
The common process of manufacturing K417G consists of vac- system, which excludes the influence of other factors. The effects of
uum induction melting (VIM) and then casting into turbine blades. cooling rate after pouring on the microstructures, microsegregation
The structure of turbine blade is complex and the thickness in dif- and mechanical properties of K417G superalloy were studied.
ferent parts is not the same [8]. During the solidification of melt,
the difference of thickness leads to different cooling rate [9]. Vari-
ous cooling rates result in the differences on the diffusion of alloy 2. Experimental
https://doi.org/10.1016/j.jmst.2017.03.023
1005-0302/© 2017 Published by Elsevier Ltd on behalf of The editorial office of Journal of Materials Science & Technology.
812 L. Gong et al. / Journal of Materials Science & Technology 34 (2018) 811–820
Table 1 homogenize the melt and then poured into the preheated mould.
Chemical compositions of K417G superalloy (wt%).
The pouring temperature was 1426 ◦ C. Molten alloys came into the
Ni C Cr Co Mo Al Ti V Zr B mould shell from the pouring gate P, flowed through the runners
Bal. 0.166 9.37 9.65 3.08 5.21 4.56 0.71 0.086 0.023 and the sprues, and then simultaneously filled into the specimen
A, B and C from the bottom of the sprues. After kept for 5 min,
the mould was removed from the vacuum induction furnace. In
the next day, the rods were removed from the sandbox. In theory,
there are three different cooling rates corresponding to specimen
A–C. The travel distance of the melt from the pouring gate to the
specimen A–C is the same. However, as shown in Fig. 1(b), spec-
imen A is the nearest to the furnace wall, C is the farthest and B
is in the middle. Since the room temperature was about 25 ◦ C and
the furnace wall was cold, it was easy for specimen A to transport
heat outside. Thus, specimen A should have the fastest cooling rate,
while C has the slowest. In order to trace the temperature during
casting, the B-type thermocouples were placed in the midsection of
specimen A–C (as shown in Fig. 1(a)). The temperature-time curves
were recorded by KSL/A-16EM1V0 temperature recorder during
the casting process.
The rod specimens were machined into gauge of
5 mm × 25 mm for high temperature tensile test and stress
rupture test. High temperature tensile test was performed at
900 ◦ C on WDW-T100 test machine with the initial displacement
speed of 0.15 mm min−1 , and then increasing to 3 mm min−1 after
yielding. Rupture test was performed at 950 ◦ C with the stress of
235 MPa on RDL-50 test machine.
Metallographic examinations were made on the longitudinal
section both at the screw position and the gauge position of the
high temperature tensile specimens. The samples were observed
by Olympus optical microscopy (OM) and FEI XL-30FEG scanning
electron microscopy (SEM). To quantitatively determine the vol-
ume fraction of the phase, the / eutectic and cast porosity, 20
images captured at different areas of each specimen were needed
by Sisc IAS image analysis system, and the average was taken. 100
particles were selected randomly in the SEM images and measured
to confirm the size of phase. The element concentrations and
distribution on the un-etched samples were investigated by JEOL
JXA8530F electron probe microanalysis (EPMA). Three points at the
dendrite core and the interdendritic region were selected randomly
in each sample and the average was taken. The samples were pre-
pared by jet-beam electro-polishing in a solution of 10% perchloric
acid and 90% ethanol at about −20 ◦ C, and then observed on FEI G2
20 transmission electron microscopy (TEM). The fracture surfaces
at 900 ◦ C tensile tests with various cooling rates were observed by
scanning electron microscopy (SEM) after ultrasonic cleaning.
Table 2
Element segregation analysis of different cooling rates (v) between dendrite core
and interdendritic regions.
Sample v (◦ C s−1 ) V Co Al Cr Mo Ti
3.3. Microstructure
Fig. 4. Microstructure at gauge position of high temperature tensile specimens with different cooling rates: (a, b) specimen A, 1.42 ◦ C s−1 ; (c, d) specimen B, 1.06 ◦ C s−1 , (e, f)
specimen C, 0.84 ◦ C s−1 .
Fig. 5. OM images showing secondary dendrite arm spacing () for specimen A (a), specimen B (b) and specimen C (c) with cooling rates of 1.42 ◦ C s−1 , 1.06 ◦ C s−1 and
0.84 ◦ C s−1 , respectively.
Table 3
Microstructure features at gauge position of specimens under different cooling rates.
Sample v (◦ C s−1 ) (m) Size of phase (nm) Volume fraction of phase (%) Size of / Volume fraction Volume fraction
eutectic (m) of / eutectic of cast porosity
(%) (%)
A 1.42 44.3 ± 0.3 521 ± 16 550 ± 11 63.3 ± 0.4 64.0 ± 0.8 31.7 ± 2.2 6.0 ± 1.3 0.24 ± 0.1
B 1.06 48.7 ± 0.3 569 ± 11 601 ± 15 63.9 ± 0.8 64.7 ± 0.6 32.2 ± 2.3 5.6 ± 1.3 0.25 ± 0.1
C 0.84 54.3 ± 0.8 612 ± 19 640 ± 9 64.7 ± 0.5 65.5 ± 0.6 41.3 ± 4.9 4.7 ± 1.2 0.25 ± 0.1
L. Gong et al. / Journal of Materials Science & Technology 34 (2018) 811–820 815
Fig. 6. Morphologies of phases in dendrite (a, c, e) and interdendrite (b, d, f) for specimen A (a, b), specimen B (c, d) and specimen C (e, f) with cooling rates of 1.42 ◦ C s−1 ,
1.06 ◦ C s−1 and 0.84 ◦ C s−1 , respectively.
of the phase in the interdendrite are slightly larger than those in [19]. At higher cooling rate, the shorter diffusion time may weaken
the dendrite. the effect of back-diffusion, and Al and Ti have insufficient time to
To better analyze the / eutectic, the samples were electrolyt- dissolve into matrix and carbides. The enrichment of Al and Ti in
ically etched with 10% phosphoric acid. As shown in Fig. 7, most the liquid would lead to more / eutectic. Therefore, the volume
of the / eutectic distributed at dendrite boundaries, and the fraction of the / eutectic is relatively larger with higher cooling
micro-porosities and carbides could be generally observed nearby, rate. On the other hand, the lower cooling rate leads to longer diffu-
which indicated that the / eutectic were formed during the last sion distance, so Al and Ti tend to gather together. Therefore, larger
stage of solidification. 10 images were measured at each sample / eutectic will precipitate there.
and the results were listed in Table 3. The average size of the / K417G is subjected to forming cast porosity because of its wide
eutectic varied from 31.7 m to 41.3 m and the average volume solidification range. As shown in Fig. 4, the micro-porosities were
fraction varied from 6.0% to 4.7%. It indicates that the volume frac- mostly presented in the interdendritic regions or grain boundaries.
tion of the / eutectic tends to be smaller and the size is larger From quantitative calculation listed in Table 3, the volume frac-
with relatively lower cooling rate. The formation of the / eutec- tions of cast porosity with different cooling rates were 0.24%, 0.25%
tic is strongly related to the microsegregation. The degree of the and 0.25%, respectively. It can be seen that the volume fraction of
microsegregation is greatly influenced by the back-diffusion in the the micro-porosity had a slight increase at lower cooling rate. The
solidified metal, and there are two factors that play a significant extent of the micro-porosity is strongly related to the solidification
part in this diffusion: the diffusion distance and the diffusion time parameters, such as grain size, precipitation and development of
816 L. Gong et al. / Journal of Materials Science & Technology 34 (2018) 811–820
Fig. 7. Morphologies and distribution of / eutectic specimen A (a, b), specimen B (c, d) and specimen C (e, f) at low (a, c, e) and high (b, d, f) magnification with cooling
rates of 1.42 ◦ C s−1 , 1.06 ◦ C s−1 and 0.84 ◦ C s−1 , respectively.
Fig. 8. Morphologies and distribution of the carbides for specimen A (a), specimen B (b) and specimen C (c) with cooling rates of 1.42 ◦ C s−1 , 1.06 ◦ C s−1 and 0.84 ◦ C s−1 ,
respectively.
secondary phase, element segregation, temperature gradient and These three different cooling rates have no significant effect on
solidification velocity[20,21]. In present study, lower cooling rate the morphology and distribution of carbides in K417G superalloy.
leads to more serious segregation, which results in the precipitation As shown in Fig. 8, the carbides showed blocky and rod-like shape
and development of the secondary phases. They serve as bridging and they mainly distributed in dendrite boundaries or near the /
obstacles in the dendritic regions and hinder the smooth flow of eutectic region. From the energy spectrum analysis (Fig. 9), the
feed metal [22,23], and thus more micro-porosities would gener- rod-like and blocky carbides are rich in Mo and Ti. As illustrated
ate. However, the variation range of cooling rate in this work is not in Fig. 10, the blocky carbide is of fcc structure with the lattice con-
very large, so the volume fraction of cast porosity varies slightly. stant a of 0.429 nm, which falls between 0.4273 (MoC) and 0.4327
L. Gong et al. / Journal of Materials Science & Technology 34 (2018) 811–820 817
Fig. 10. TEM image and SAED pattern of MC carbide in specimen C with cooling rate
of 0.84 ◦ C s−1 .
Fig. 9. SEM images of carbides (a) and EDS analysis of different areas (b, c).
Table 4
Microstructure features at screw position of specimens under different cooling rates.
Sample v (◦ C s−1 ) (m) Size of phase (nm) Volume fraction of phase (%) Size of / Volume fraction Volume fraction
eutectic (m) of / eutectic of cast porosity
(%) (%)
A 1.42 47.1 ± 0.5 565 ± 12 589 ± 17 64.3 ± 0.4 64.9 ± 0.6 33.2 ± 2.4 4.9 ± 1.2 0.21 ± 0.1
B 1.06 50.9 ± 0.7 594 ± 15 622 ± 10 64.9 ± 0.7 65.7 ± 0.7 34.7 ± 2.8 4.8 ± 0.9 0.24 ± 0.2
C 0.84 54.7 ± 0.3 627 ± 10 653 ± 13 65.9 ± 0.6 66.2 ± 0.9 44.4 ± 3.7 4.7 ± 0.5 0.24 ± 0.1
Table 5
High temperature tensile properties and stress rupture properties of K417G superalloy with various cooling rates.
Sample v (◦ C s−1 ) Ultimate tensile strength (MPa) Elongation (%) Reduction of area (%) Rupture life (h)
Fig. 13. SEM images of fracture surfaces after tensile test at 900 ◦ C for specimen A (a, b), specimen B (c, d) and specimen C (e, f) at low (a, c, e) and high (b, d, f) magnification
with cooling rates of 1.42 ◦ C s−1 , 1.06 ◦ C s−1 and 0.84 ◦ C s−1 , respectively.
Fig. 14. OM images of fracture surfaces after tensile tests at 900 ◦ C for specimen A (a), specimen B (b) and specimen C (c) with cooling rates of 1.42 ◦ C s−1 , 1.06 ◦ C s−1 and
0.84 ◦ C s−1 , respectively.
shear stress, the slip and deformation in the grain boundary and the because of stress concentration, which leads to the formulation and
interdendrite lead to microcracks. The expansion of microcracks propagation of microcracks, so the increased volume fraction of
along the grain boundary and the interdendrite leads to the fracture / eutectic in the grain boundary and the interdendritic region
of materials. Therefore, with the cooling rate increasing, the volume results in low ductility property of K417G alloy.
fraction of / eutectic increases a lot, which would hinder the The favorable stress rupture life mainly depends on the
movement of dislocations. Thus, a larger deformation will generate increased volume fraction of phase [34]. Specimen C with the
820 L. Gong et al. / Journal of Materials Science & Technology 34 (2018) 811–820
cooling rate of 0.84 ◦ C s−1 has relatively larger volume fraction of Acknowledgements
phase, so it results in a longer rupture life. However, this improve-
ment is not obvious because there are small differences in the The authors thank Jiangsu Tunan Alloy Co., Ltd for providing
volume fraction of phase with different cooling rates. alloy and their assistance on the remelting and cast procedures.
The / eutectic is a phase with lower strength and is prone to Prof. Shunnan Zhang is especially acknowledged for his advice on
form cracks [20,35]. Moreover, / eutectic contains an amount the solidification experiments.
of formation elements, such as Al and Ti, which results in a
decreased volume fraction of phase [20,35]. Therefore, / References
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