Interfacial Reaction Between Nickel-Based Superalloy K417G and Oxide Refractories
SONG Qingzhong1,2, QIAN Kun1,3, SHU Lei1,3, CHEN Bo1,3(), MA Yingche1,3, LIU Kui1,3
1.Institute of Metal Research, Chinese Academy of Sciences, Shenyang 110016, China 2.School of Metallurgy, Northeastern University, Shenyang 110819, China 3.Shi -changxu Innovation Center for Advanced Materials, Institute of Metal Research, Chinese Academy of Sciences, Shenyang 110016, China
Cite this article:
SONG Qingzhong, QIAN Kun, SHU Lei, CHEN Bo, MA Yingche, LIU Kui. Interfacial Reaction Between Nickel-Based Superalloy K417G and Oxide Refractories. Acta Metall Sin, 2022, 58(7): 868-882.
High-performance nickel-based superalloys are highly desired in the aerospace industry. A drawback of vacuum induction melting for processing nickel-based superalloys is that oxide refractories contaminate the molten alloy through crucible-melt interaction. Therefore, crucibles used for producing nickel-based superalloys should be carefully selected to avoid melt contamination. In this study, the interfacial reaction between a molten nickel-based superalloy (K417G) and various oxide refractories, including Al2O3, CaO, MgO, ZrO2 + 12%Y2O3 (mass fraction) (Y-PSZ), ZrO2 + 20%CaO (CSZ), and Y2O3, formed by cold isostatic pressing was investigated at 1600oC by XRD, SEM, and EDS. The effects of the oxide crucibles on the impurity contents of K417G were also evaluated. The results show that physical erosion is the primary mechanism of the interaction between Al2O3 crucibles and alloy melt. The readily detached Al2O3 particles formed inclusions in the alloy. The Ca3Al2O6 liquid phase generated at the melt-crucible interface promoted wettability between the alloy and CaO crucible, resulting in a high adhesion at the interface. The reaction of the MgO crucible with Al in the alloy resulted in the formation of MgAl2O4 at the melt-crucible interface, which subsequently entered the alloy to form inclusions. Al2O3 was generated at the Y-PSZ-crucible-alloy interface. However, there was no corrosion of Al2O3 in the Y-PSZ crucible, indicating the crucible exhibits excellent corrosion resistance to Al2O3 slags. The interaction between the CSZ crucible and alloy melt generated a CaAl2O4 liquid phase, making the crucible unstable to dissolve into the alloy. An Al2Y4O9 reaction layer is mainly formed at the Y2O3-crucible-alloy interface. The dissolution of Y2O3 into the alloy melt was high compared to that of other oxide refractories. The melt-crucible interaction also significantly affected the oxygen content of K417G. The oxygen concentration of the alloy fused by CaO, Y2O3, and Y-PSZ crucibles did not increase, whereas that of the alloy melted in CSZ, MgO, and Al2O3 crucibles increased from 0.0007% to 0.0011%, 0.0034%, and 0.0135%, respectively.
≥ 98.5, Fe ≤ 0.005, Ba ≤ 0.003, Cl- ≤ 0.07, SO ≤0.05, Pb ≤ 0.005, Loss ≤ 4.5,
Y2O3
≥ 99.99, Loss ≤ 0.01
ZrO2
≥ 99.0, Fe2O3 ≤ 0.005, MgO ≤ 0.05, CaO ≤ 0.05, TiO2 ≤ 0.005, SiO2 ≤ 0.01, Loss ≤ 1
Table 1 Purities of raw materials for manufacturing oxide crucibles
Crucible
Composition
Pressure
Sintering temperature
Apparent porosity
Bulk density
(mass fraction)
MPa
℃
%
g·cm-3
Al2O3
100%
280
1680
1.26
3.76
CaO
100%
280
1680
1.23
3.00
MgO
100%
280
1680
1.23
3.40
Y-PSZ
12%Y2O3 + 88%ZrO2
280
1680
15.00
4.94
CSZ
20%CaO + 80%ZrO2
280
1680
28.00
3.50
Y2O3
100%
280
1680
21.50
3.94
Table 2 Process parameters forming oxide crucibles, apparent porosity, and bulk density
Fig.1 Schematic diagram of experiment equipment
Fig.2 XRD spectra of various oxide crucibles after sintering (a) Al2O3 and MgO (b) CaO and Y2O3 (c) Y-PSZ and CSZ (m—monoclinic, t—tetragonal, c—cubic)
Fig.3 Macromorphology of nickel-based superalloy K417G smelted by Al2O3 crucible
Fig.4 Al2O3 inclusions flowed at the liquid surface
Fig.5 SEM image (a) and EDS mappings (b-f) of the interface between Al2O3 crucible and nickel-based superalloy K417G
Location
O
Al
Ca
Mg
Ti
Ni
A
54.27
41.12
3.31
0.45
0.30
0.55
B
55.79
44.21
0.00
0.00
0.00
0.00
Table 3 Chemical compositions of the interface between Al2O3 crucible and K417G alloy in Fig.5a by EDS analysis
Fig.6 SEM image (a) and EDS mappings (b-f) of the interface between CaO crucible and nickel-based superalloy K417G
Location
O
Al
Ca
Ti
V
Co
Ni
C
49.39
20.04
30.15
0.04
0.07
0.07
0.24
D
64.92
0.00
34.97
0.08
0.00
0.00
0.03
Table 4 Chemical compositions of the interface between CaO crucible and K417G alloy in Fig.6d by EDS analysis
Fig.7 Macromorphology of nickel-based superalloy K417G smelted by CaO crucible
Fig.8 SEM image (a) and EDS mappings (b-f) of the interface between MgO crucible and nickel-based superalloy K417G
Location
O
Al
Mg
Cr
Ni
E
50.91
32.73
16.12
0.09
0.15
F
43.41
0.17
56.21
0.08
0.13
Table 5 Chemical compositions of the interface between MgO crucible and K417G alloy in Fig.8a by EDS analysis
Fig.9 MgAl2O4 inclusions flowed at the liquid surface
Fig.10 SEM image (a) and EDS mappings (b-f) of the interface between Y-PSZ crucible and nickel-based superalloy K417G
Location
O
Al
Zr
Y
Ti
Cr
Co
Ni
G
57.99
41.78
0.00
0.00
0.11
0.00
0.00
0.12
H
62.33
0.47
31.26
5.15
0.10
0.24
0.11
0.34
Table 6 Chemical composition of the interface between Y-PSZ crucible and K417G alloy in Fig.10a by EDS analysis
Fig.11 Al2O3 inclusions flowed at the liquid surface smelted by Y-PSZ crucible
Fig.12 SEM images (a) and EDS mappings (b-f) of the interface between CSZ crucible and nickel-based superalloy K417G
Location
O
Al
Ca
Zr
Ti
Cr
Co
Ni
I
56.33
0.27
0.20
39.75
0.08
0.42
0.45
2.50
J
60.28
0.10
0.22
38.39
0.07
0.00
0.00
0.95
K
50.61
27.25
16.95
4.54
0.14
0.01
0.17
0.34
L
70.04
0.00
5.23
24.74
0.00
0.00
0.00
0.00
M
63.43
23.77
11.51
1.29
0.00
0.00
0.00
0.00
N
60.07
0.00
17.93
21.32
0.27
0.00
0.00
0.00
O
61.94
0.00
6.65
31.41
0.00
0.00
0.00
0.00
Table 7 Chemical composition of the interface between CSZ crucible and K417G alloy by EDS analysis (See points in Figs.12-14)
Fig.13 Backscattered electron (BSE) image (a) and EDS mappings (b-d) of CSZ crucible after smelting nickel-based superalloy K417G
Fig.14 BSE image of original micromorphology of CSZ crucible
Fig.15 Macromorphology of nickel-based superalloy K417G smelted by CSZ crucible
Fig.16 SEM image (a) and EDS mappings (b-f) of the interface between Y2O3 crucible and nickel-based superalloy K417G
Fig.17 BSE images of interface between Y2O3 crucible and K417G alloy (a) and K417G alloy (b) smelted by Y2O3 crucible (Insets are EDS mappings of segregation regions of Y inside K417G alloy)
Location
O
Al
Y
Ti
Cr
Co
Ni
P
57.23
13.45
28.70
0.15
0.04
0.06
0.37
Q
56.05
0.00
43.82
0.00
0.03
0.05
0.05
Table 8 Chemical compositions of the interface between Y2O3 crucible and K417G alloy in Fig.17a by EDS analysis
Crucible
O
Al
Ca
Mg
Zr
Y
Al2O3
0.0135
5.25
-
-
-
-
CaO
0.0006
-
0.0010
-
-
-
MgO
0.0034
-
-
0.0090
-
-
Y-PSZ
0.0008
-
-
-
0.068
< 0.0010
CSZ
0.0011
-
0.0008
-
1.760
-
Y2O3
0.0007
-
-
-
-
0.0150
Table 9 Impurity element contents of nickel-based superalloy K417G after melting
Fig.18 Relationships between the formation Gibbs free energy (ΔGθ ) of various oxide materials and temperatures
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