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Phase Transformations and Grain Growth Behaviors in Superalloy 718
Phase Transformations and Grain Growth Behaviors in Superalloy 718
PII: S0925-8388(17)34109-9
DOI: 10.1016/j.jallcom.2017.11.327
Reference: JALCOM 44020
Please cite this article as: J.J. Ruan, N. Ueshima, K. Oikawa, Phase transformations and grain
growth behaviors in superalloy 718, Journal of Alloys and Compounds (2017), doi: 10.1016/
j.jallcom.2017.11.327.
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1473 K for 170 mins 1473 K for 170 mins
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8 mm 4 mm Thermo-Cal pinning controller was
endothermic
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was introduced. identified.
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Atmosphere : argon gas flow Mechanism for
The microstructure of the alloy m=4 15.5
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grain growth
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for DSC measurement -2.0
NbC 14.5
ln(K1T/CmNb )
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γ 1473 K
-3.0 1373 K
D
13.5
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R2=0.97
ln(dG/dt)
exothermic
-4.0
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4 mm TiN 12.5 Q=417 kJ/mol
1555 K
C
-5.0 m=4
AC
ing 1495 K 11.5
Heat m=3
1323 K
1423 K 0.68 0.70 0.72 0.74 0.76
1073 1173 1273 1373 1473 1573 -6.0 m=2 1/T, 10-3 K-1
4.5 4.9 5.3 5.7 6.1
Temperature / K lnG
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Phase transformations and grain growth behaviors in superalloy 718
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Abstract: The phase transformation and grain growth behaviors of commercial
Ni-Fe-base superalloy 718 at 1323, 1373, 1423 and 1473 K were investigated through
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DSC and SEM methods. The transformation temperatures of γ + NbC → L and
γ → L were determined as 1495 and 1555 K, respectively, and TiN was shown to
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gradually dissolve into the formed L. The pinning effect caused by Nb-rich carbide
(NbC) and Ti-rich nitride (TiN) was observed, and the mean size of the grains
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increased with holding time at each temperature. The grain growth exponent, m, was
the precipitate through grain boundary diffusion. The grain boundary diffusion of Nb
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and N was confirmed to control the coarsening of NbC and TiN, respectively. The
major factor for γ grain growth was confirmed to be the coarsening of NbC, and the
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activation energy for grain growth was calculated as 417 kJ·mol-1. The equations for
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(1373 K), G4-G04=2.01×106×t (1423 K) and G4-G04=3.89×106×t (1473 K), for all
four temperatures respectively. The predicted grain growth curves were in good
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1. Introduction
its ability to maintain its attractive mechanical properties for lengthy periods of time
In addition to this, due to the sluggish precipitation of the main strengthening phase γ''
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(DO22-ordered crystal structure), superalloy 718 also shows good weldability. It has
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been confirmed that the weld residual stresses are able to be released before the
precipitation of γ'', then the strain-age cracking usually occurred during followed
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aging heat-treatment can be resisted [1]. Thus, superalloy 718 is extensively used in
the gas turbine industry for rotating disks and shaft components, etc [1, 4].
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Apart from the coherent dispersion strengthening caused by the metastable
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coherent γ'' phase, another metastable L12-ordered γ' with a smaller volume fraction
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than that of γ'' also makes a small contribution to the reinforcement of superalloy 718
[1, 4-11]. The other phases reported in superalloy 718 are orthorhombic DOa-ordered
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close-packed Laves-C14 [4, 12, 16-18], discrete Nb-rich MC-type carbides (NbC) [4,
9, 12, 16, 19] and Ti-rich MN-type nitrides (TiN), etc [19-23].
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The microstructure, and particularly the size of the grains in the matrix, largely
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determines the properties of the superalloys [24-26]. For instance, a large grain size
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has been shown to slow the crack growth rate in superalloy 718 under cyclic loading
to occur. To date, investigations into the grain growth behavior have mainly been
focused on nanocrystalline [27] and hot deformed [28-30] superalloy 718. However,
rather insufficient data regarding the grain growth of bulk superalloy 718 under
2
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provided by Huda et al. [31-32] shows a considerable scattering when subject to the
mathematic calculations used in the present work: this is particularly invalid for lower
temperatures (1323 and 1373 K). This scatter is discussed in section 3.2. Therefore,
the main objective of the present work is to obtain data related to the growth kinetics
of the matrix γ during isothermal holding at temperatures higher than the solvus of the
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δ-Ni3Nb phase, and to provide essential information for the prediction of the
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microstructure evolution of superalloy 718.
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2. Experimental details
The material used in the present work was provided by the Hitachi Metals
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company, and its composition is listed in Table 1. Samples with the dimensions of
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10mm × 5mm × 1.5mm were cut from the as-received alloy, polished using abrasive
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paper, and then sealed in the quartz capsules backfilled with high-purity argon after
influences of γ', γ'' and the δ-Ni3Nb phases on γ grain growth. The samples were
quenched into ice water after heat-treatment. Details of the heat-treatments performed
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determine the appropriate annealing temperature for the present work. Microstructure
(FE-SEM), and the chemical compositions of carbide and nitride were analyzed by the
energy dispersive spectrometer (EDS) equipped on the FE-SEM. The alloys were
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The commonly used two-dimensional microstructure was adopted instead of the
calculating the grain size [33]. Since the microstructures were simple, with only a
small amount of precipitates (NbC and TiN) [34], the Jeffries’ (or Planimetric)
procedure was considered suitable for measuring the mean grain size from the
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FE-SEM images. In the Jeffries’ method, the average area, Am, is calculated by
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dividing the total area by the number of grains counted (N): each grain clearly inside
the test area (a circle in the present work) was counted as 1 while those which were
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partially inside the test area were counted as 0.5 [34]. Meanwhile, the mean grain size
was represented by the diameter G of an equivalent circle with same area Am [33-36].
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3. Results and discussion
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the tiny precipitates can be observed. Because the as-received alloy was taken from a
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1(b) are the γ', γ'' and δ-Ni3Nb phases. The Nb-rich carbide NbC (white contrast) and
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the Ti-rich nitride TiN [19, 21] (grey contrast phase in Figure 1(c)) are confirmed by
the energy dispersion spectrum (EDS) results, as shown in Figure 1(d). The
researchers [20-22] with part of the NbC phase nucleating on pre-existing TiN.
Importantly, though the influence of possible γ', γ'' and δ-Ni3Nb on γ grain growth can
be avoided, the high solvus temperature of NbC and TiN means their influence on γ
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grain growth must be considered.
The DSC heating curve obtained from the alloy annealed at 1473 K for 170 mins
is shown in Figure 2(a), where two transition peaks, 1495 and 1555 K, are identified.
The microstructure of the alloy before the DSC test is shown in Figure 2(b): the white
area is the NbC phase and the grey area is the TiN phase.
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In order to reveal the phase transitions during heating process, the alloys were
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heated at the same heating rate (10 K/min) as that of the DSC test, and then quenched
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magnification image obtained from the alloy quenched from 1537 K is shown in
Figure 3(a). The decomposing TiN and NbC phases are clearly visible in this sample,
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as shown in Figures 3(b) and (c), respectively, and the eutectic microstructure derived
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from the cooling of the liquid phase during quenching is also evident. Thus, it was
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eutectic (γ/ NbC) (derived from the liquid phase (L) after water quenching). The
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eutectic microstructure (γ/ NbC) in superalloy 718 was also observed by Knorovsky
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[16]. The melting of the matrix γ in the alloy quenched from 1580 K is clear from the
image in Figure 3(d). The solidus temperature of the superalloy 718 was reported as
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1500 and 1593 K by Eiselstein [37] and Knorovsky [16], respectively. The melting
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temperature of the matrix γ indicated in Figure 2(a) (1555 K) is between these two
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the variation in the solidus temperature is reasonable. The decomposing TiN, eutectic
(γ/ NbC) and dendrite γ are also clear in this sample, as shown in Figures 3(e) and (f),
Since decomposing TiN is found near the eutectic microstructure (Figures 3(b)
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and (e)) for both quenching temperatures (1537 and 1580 K), it can be assumed that
TiN gradually dissolved into the liquid phase as the temperature increased. This is in
good agreement with the finding by Cockcroft and Mitchell et al. [20-21] that the
Considering the high N content (65 ppm) in the present alloys (Table 1), and the
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solubility of N in superalloy 718 at 1700 K, calculated by Cockcroft et al. [20] to be ~
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38 ppm, it is believed that some pockets of TiN exist above the liquidus temperature
even though most of the TiN has dissolved into the liquid phase. As such, the peak
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located at 1495 K in Figure 2(a) can be largely attributed to the formation of the liquid
phase due to the reaction between NbC and the γ phases, while the peak at 1555 K can
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be attributed to the melting of the remaining matrix γ.
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A total of four annealing temperatures, 1323, 1373, 1423 and 1473 K, were
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chosen to investigate grain growth behavior in the absence of influence from γ', γ'',
δ-Ni3Nb and the liquid phases. The holding times selected ranged from 0 to 281
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minutes after solution heat-treatment. The microstructures of the alloys after solution
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Diffraction) grain maps. The mean grain sizes of the alloys heat-treated at 1323, 1373,
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1423 and 1473 K were measured as 97, 147, 162 and 221 µm, respectively, and are
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listed in Table 2. In the sample annealed at 1473 K for 170 mins after solution
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heat-treatment, grain boundary pinning microstructures resulting from the TiN and
The grain growth curves in Figure 6 indicate an increase in the grain size as the
growth rate slowed down with longer annealing-time at each temperature. The
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kinetics of isothermal grain growth can be described by the parabolic equation
G − G = KV σt (1)
where G is the average grain diameter; G0 is the mean grain size at t=0; σ is the grain
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temperature related parameter.
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This parabolic equation (Equation (1)), however, tends to be applied to the pure
single phase grain growth since it only considers the driving force caused by the
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reduction of the total amount of grain boundary energy and does not consider other
factors affecting grain growth, such as the solute atoms, solute segregation,
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precipitates or texture [38-39]. Thus, a more general modified equation based on the
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parabolic equation, power law, was proposed as a mathematical expression of
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G − G = K t (2)
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boundary [39-40]. It should be noted that the m value is also affected by the void size
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and distribution, solute and segregation, the size and distribution of the second phase,
In this study, the average grain diameter of the alloys after solution
obtained.
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dG K
( ) = + (1 − m)G (3)
dt m
dG G − G
= ;
dt t − t
dG 1 dG dG"
= ∗ + ;
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dt 2 dt dt "
dG" 1 dG dG#
= ∗ + ;
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dt " 2 dt dt #
.
.
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.
dG% G% − G%&
=
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dt % t % − t %&
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The m and K1 values at each temperature are determined from the linear
regression of the plot of ln(dG/dt) versus lnG displayed in Figure 7. A fixed m value
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[39-40], and K1 is calculated as 0.10 × 106 (1323 K), 0.49 × 106 (1373 K), 2.01 × 106
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(1423 K) and 3.89 × 106 (1473 K) µm4·s-1, respectively. It was not possible to
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describe the present experimental data with other m values, such as 2 or 3, as can be
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seen in Figure 7. The pinning microstructures observed in Figures 5(a)-(b) confirm the
matrix. The plots in Figure 8 were computed by the same methods used in the present
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work using the grain growth data of superalloy 718 provided by Huda et al [31-32].
While m values of 3.76 (1323 K), 3.92 (1373 K), 3.72 (1423 K) and 3.61 (1473 K)
were obtained, it should be noted that these plots show poor coefficients of
growth curves were obtained, and are displayed in Figure 9 with the measured grain
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size. It can be seen that the predicted data is in good agreement with the experimental
data.
The relationship between the grain size of the matrix and particle size was
studied by many researchers [41-43], and can be finally described by Equation (4)
G K
= ) (4)
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r f
where r and f are the size and volume fraction of second-phase particles,
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respectively, K2 and k are constants for a given system. The value of f does not
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change during Ostwald ripening. The relationship between particle size and heating
time can be expressed in Equation (5) [44] if the Ostwald ripening of particle is
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limited by the grain boundary diffusion.
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8 γC. ωv D·2
r# − r# = t (5)
9 ABRT
where r0 is the initial size of the second-phase particles; 8 is the interfacial energy
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atoms in the boundary without the influence of precipitates; ω is the thickness of the
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grain boundary; νm is the molar volume of the particle; Dg·b is the grain boundary
diffusion coefficient; and A and B are constants. By integrating Equations (2), (4) and
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C. D·2
C
K = K " (6)
T
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:;=< >ω?<@
where K " = and is constant for the same particle, and Dg·b is described in
AB=C DEF
Equation (7)
Q·2
D·2 = D exp(− ) (7)
RT
where D0 is the diffusion coefficient at infinite temperature, and Qg·b is the activation
controller element for the coarsening of the precipitate. Ideally, the grain boundary
diffusion data of Nb, Ti, C and N in superalloy 718 would be used to determine the
diffusion controller in the present work due to the pinning microstructures seen in
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coefficients of Nb [45] and Ti [46], and the impurity-diffusion coefficient of C [47] in
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Ni were used, and the related data is listed in Table 3 where the data related to
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crystal structure) are also provided. The diffusion coefficients were calculated by
Equation (8) using the data provided in Table 3, and are listed in Table 4.
D = D exp(−
Q
) U (8)
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RT
where D is the diffusion coefficient, and Q is the activation energy for diffusion. The
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relationship between the diffusion coefficient and temperature are also plotted in
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Figures 10(a)-(b): the inter- (Nb and Ti in Ni) and impurity-diffusion coefficients (C
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in Ni, C and N in γ-Fe) clearly increase with rising temperature. In Table 4, it can be
in Fe even though they show the same order of magnitude (-11). Thus, because both C
and N are interstitial atoms, it is reasonable to assume the same tendency for the
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The equilibrium molarity (Cm) of the solute atoms Nb, C, Ti and N in the matrix
γ was taken into account due to the lack of C. , despite the difference between them.
by the Thermo-Calc software [50] using the Ni-Data database [51] and the lattice
constant of the matrix γ, the Cm for the solute atoms Nb, C, Ti and N in the matrix γ
can be calculated. In the investigation performed by Dehmas et al. [3], the lattice
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constant of the matrix γ slightly decreases with the loss of Nb in the matrix γ caused
by the precipitation of the δ-Ni3Nb phase. The difference between the lattice constant
of the matrix γ without the δ-Ni3Nb phase and that of the matrix γ which contains a
small amount of the δ-Ni3Nb phase is negligible for the calculation of the matrix
molar volume in the present work. As such, the lattice constant of the matrix γ (3.604
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Å) with the lowest volume fraction of the δ-Ni3Nb phase in the results reported by
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Dehmas et al. [3] was used for all the temperatures investigated in the present work.
The calculated Cms for the solute atoms Nb, C, Ti and N in the matrix γ and the
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related data are listed in Table 5.
The products of C and D for the solute atoms Nb, C, Ti and N were calculated
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using the data listed in Tables 4-5, as seen in Table 6. Note that the DR2 Q% RQ R2
L%MNO&PQBB. ·C is
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lower than DVLSTOQMU&PQBB.
Q% RQ V
·C by about one order of magnitude, while DWQ Q% RQ WQ
L%MNO&PQBB. ·C
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exceeds than DR Q% XN R
LSTOQMU&PQBB. · C by about one order of magnitude among the
temperatures investigated. This suggests that Nb is the controller for the Ostwald
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ripening of NbC, and that N is the controller for the Ostwald ripening of TiN.
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The number densities of the NbC and TiN in the solution-treated samples are
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necessary for determining the main pinning phase on the matrix γ grain boundary
during the heating process. However, because they sparsely distributed in the sample,
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it is difficult to count them. The molar percentage of NbC and TiN in the alloys after
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solution heat-treatment is believed to be close to that of NbC and TiN in the alloys
under equilibrium because of the small size of the pre-existent precipitates indicated
in Figure 1(b). Through the molar percentage of NbC and TiN in the matrix γ
calculated by the Thermo-Calc software [50] using the Ni-Data database [51] and the
lattice constant of these phases, the volume of NbC and TiN in the alloy with 1 mol
can be obtained. The lattice constants of NbCx and TiNx were calculated using the
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lattice constants obtained by Storms [52] (aNbCx
N/Ti, respectively, and was calculated through the molar percentage of the solutes in
NbCx and the solutes in TiNx provided by the Thermo-Calc software [50] using the
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Ni-Data database [51]. The calculated volumes of NbC and TiN in the alloy with 1
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mol are listed in Table 7 where the related data is also displayed. The ratios of
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accept the results obtained by other researchers [20-22] that the TiN provides the
nucleation site for the precipitation of NbC, it is reasonable to assume that the number
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density of NbC is higher than that of TiN. This speculation agrees well with the
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conclusion derived from the present volume ratio calculation on NbC and TiN that the
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number density of NbC is higher than that of TiN if the mean sizes of these two
phases are close. This further indicates that the NbC is the main controller for γ grain
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K T Q·2
= K # − (9)
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C. RT
where K4=K3·D0. As mentioned above, the γ grain growth is mainly controlled by the
C
coarsening of NbC, while the solute Nb is the controller for the coarsening of NbC,
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R2
therefore, the equilibrium molarity C of the Nb in the matrix γ was adopted for the
calculation of the activation energy for γ grain growth. Then, the relationship between
R2
ln(K1T/C ) and 1/T was plotted, as shown in Figure 11 where Qg·b is 417 kJ·mol-1.
4. Summary
The phase transitions during the heating process and grain growth behaviors of
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the commercial Ni-Fe-based superalloy 718 were investigated, and the power law was
introduced for its mathematical expression. The predicted curve fits the present
experimental data well. The main experimental and calculated results can be
summarized as follows:
(1) Matrix γ starts to react with NbC to form L phase at 1495 K, and transforms
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into the L phase at 1555 K, while TiN gradually dissolves into the formed L phase.
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(2) The pinning effects caused by NbC and TiN phases on γ grain growth were
confirmed. The determined grain growth exponent m value of 4 indicates that γ grain
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growth was controlled by the Ostwald ripening of the NbC and TiN phases through
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(3) The power laws for grain growth were determined to be G4-G04=0.10×106×t
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(1323 K), G4-G04=0.49×106×t (1373 K), G4-G04=2.01×106×t (1423 K) and G4-G04
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(4) The diffusion of Nb was confirmed to control the coarsening of NbC while
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the coarsening of TiN is controlled by the diffusion of N. The coarsening of NbC was
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shown to be the largest factor controlling the γ grain growth, and the activation energy
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Acknowledgements
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This work was supported by Council for Science, Technology and Innovation
Materials for Innovation” (Unit No. B21, Development of Innovative Forging Process
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[48] J. Ågren, A revised expression for the diffusivity of carbon in binary Fe-C
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austenite, Scr. Metall., 20 (1986) 1507-1510.
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[49] P. Grieveson, E.T. Turkdogan, Kinetics of Reaction of Gaseous Nitrogen with
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Iron Part I: Kinetics of Nitrogen Solution in Gamma Iron, Trans. Metall. Soc.
United Kingdom.
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[52] E.K. Storms, N.H. Krikorian, The variation of lattice parameter with carbon
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Figure Captions
Fig. 1. BSE images (a)-(c) and energy spectrum results (d) obtained from the
as-received alloy.
Fig. 2. (a) DSC heating curve and (b) BSE image obtained from the alloy annealed at
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Fig. 3. BSE images obtained from the alloys quenched from 1537 K (a)-(c), and 1580
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K (d)-(f).
Fig. 4. EBSD grain maps with same scale obtained from the alloys after solution
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heat-treatment: (a) 1323 K; (b) 1373 K; (c) 1423 K; (d) 1473 K.
Fig. 5. BSE images obtained from the alloy annealed at 1473 K for 170 mins after
solution heat-treatment.
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Fig. 6. Measured grain size versus heating-time for each isothermal temperature.
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Fig. 8. Plots of ln(dG/dt) against lnG: calculated from the experimental data reported
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by Huda et al [31-32].
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Fig. 9. Comparisons between predicted growth curves and experimental data at each
isothermal temperature.
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Fig. 10. Plots of lnD against 1/T (a), and D against T (b).
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Table Captions
Table 1. Chemical composition of the superalloy 718 used in the present work
(mass %).
Table 3. Data relating to the inter-diffusion of Nb [45] and Ti [46] in Ni, and the
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impurity-diffusion of C [47] in Ni, C [48] and N [49] in Fe.
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Table 4. Predicted diffusion coefficients using the reported diffusion data [45-49].
Table 5. Equilibrium molarity of the solute atoms in the matrix and the related data.
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Table 6. The D·Cm of the solute atoms in the matrix.
Table 7. Volumes of the NbC and TiN phases in the alloy with 1 mol and the related
data.
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Table 1. Chemical composition of the superalloy 718 used in the present work (mass %).
Ni Fe Cr Nb Mo Ti Al Co Si
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53.8 Bal. 18.12 5.42 2.97 0.93 0.46 0.27 0.09
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Mn C Ta Zr N P B Mg S
0.07 0.025 <0.01 <0.01 0.0065 0.006 0.003 0.0013 0.0001
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Table 2. Details of the heat-treatments performed in the present work.
T/K Time for solution Mean grain diameter after Holding time for isothermal
heat-treatment / solution heat-treatment / µm heat-treatment / mins
mins
1323 15 97 0, 10, 25, 96, 165
1373 15 147 0, 10, 25, 96, 165
1423 10 162 0, 6, 23, 101, 281
1473 10 221 0, 6, 23, 101, 170
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Table 3. Data relating to the inter-diffusion of Nb [45] and Ti [46] in Ni, and the
impurity-diffusion of C [47] in Ni, C [48] and N [49] in Fe.
Inter-diffusion Impurity-diffusion
D0 / m2·s-1 Q / kJ·mol-1 D0 / m2·s-1 Q / kJ·mol-1
Nb in Ni 0.88 × 10-4 257 - -
Ti in Ni 4.1 × 10-4 275 - -
C in Ni
(Recalculated in - - 8.36 × 10-5 172
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C in Fe
(Recalculated in - - 2.34 × 10-5 148
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N in Fe
9.10 × 10-5
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the present work)
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Table 4. Predicted diffusion coefficients using the reported diffusion data [45-49].
Dinter-diffusion / 10-14 m2·s-1 Dimpurity-diffusion / 10-11 m2·s-1
T/K
Nb in Ni Ti in Ni C in Ni C in Fe N in Fe
1323 0.63 0.57 1.35 3.35 1.93
1373 1.47 1.41 2.39 5.48 3.38
1423 3.24 3.30 4.06 8.64 5.69
1473 6.77 7.25 6.65 13.21 9.24
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Table 5. Equilibrium molarity of the solute atoms in the matrix and the related data.
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Molar volume of Molar percentage of the solute atoms in the Molarity of the solute atoms in the matrix γ, Cm /
Lattice constant of
T/K
the matrix γ / Å [3]
the matrix γ / matrix γ / % [50-51] mol·m-3
m3·mol-1
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Nb C Ti N Nb C Ti N
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1323 3.27 5.02 × 10 1.09 4.99 × 10-5 1.16 × 103 1.78 3.88 × 102 1.77 × 10-2
1373 3.28 8.08 × 10-3 1.09 8.59 × 10-5 1.16 × 103 2.87 3.87 × 102 3.05 × 10-2
a=b=c=3.604 2.82 × 10-5
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1423 3.29 12.56 × 10-3 1.09 14.22 × 10-5 1.17 × 103 4.46 3.87 × 102 5.05 × 10-2
1473 3.19 19.51 × 10-3 1.07 23.10 × 10-5 1.13 × 103 6.92 3.79 × 102 8.20 × 10-2
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1323 0.73 × 10-11 0.24× 10-10 0.22 × 10-11 0.34 × 10-12
1373 1.71× 10-11 0.69× 10-10 0.55 × 10-11 1.03 × 10-12
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1423 3.77× 10-11 1.81× 10-10 1.27 × 10-11 2.87 × 10-12
1473 7.67× 10-11 4.60× 10-10 2.75 × 10-11 7.58 × 10-12
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Table 7. Volumes of the NbC and TiN phases in the alloy with 1 mol and the related data.
Molar percentage of the main solutes Molar Volume of the phases in
Molar ratio x Lattice constant (a=b=c) / Å
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Phases T/K in phases / % [50-51] percentage / the alloy with 1 mol /
[52-53] -2
Nb C Ti N C/Nb N/Ti 10 % [50-51] 10-8 m-3
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1323 50.12 45.48 0.907 4.4651 24.78 1.660
1373 49.62 45.44 0.916 4.4658 23.98 1.607
NbC
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1423 49.09 45.37 0.924 4.4665 22.87 1.533
1473 48.47 45.32 0.935 4.4673 20.44 1.371
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1323 49.19 43.75 0.889 4.2340 6.04 0.345
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1373 49.38 42.56 0.862 4.2327 6.16 0.351
TiN
1423 49.45 41.32 0.836 4.2315 6.28 0.358
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1473 49.58 39.84 0.804 4.2300 6.45 0.367
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Highlights
(1) Phase transformations and γ growth behaviors in superalloy 718 were studied;
(2) The γ grain growth curves at four isothermal temperatures were determined;
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(3) Precipitate coarsening was confirmed to control γ grain growth;
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(4) Nb and N are the controller for the coarsening of NbC and TiN, respectively;
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(5) Activation energy for γ grain growth was calculated as 417 kJ·mol-1.
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