Met. Mater. Int., Vol. 22, No. 5 (2016), pp.

789~796
doi: 10.1007/s12540-016-6305-1

High Temperature Oxidation Resistance of Ni-(5~13)Co-(10~16)Cr-(5~9)W-5Al-

(1~1.5)Ti-(3~6)Ta Alloys

Hee-Soo Kim1, Si-Jun Park2, Seong-Moon Seo3, Young-Soo Yoo3, Hi-Won Jeong3, and HeeJin Jang1,*

1
Department of Materials Science and Engineering, Chosun University, 309 Pilmundaero, Dong-gu,
Gwangju 61452, Republic of Korea
2
Multi-Material Research Center, Gwangju-Jeonnam Division, Korea Automotive Technology Institute,
Gwangju 62207, Republic of Korea
3
High Temperature Materials Group, Korea Institute of Materials Science, 797 Changwondaero,
Seongsan-gu, Changwon 51508, Republic of Korea
(received date: 4 May 2016 / accepted date: 17 May 2016)

The oxidation behavior of Ni-based superalloys was examined by cyclic oxidation tests at 850 and 1000 °C. The
present study focused on the investigation of two newly developed and three commercial alloys (GTD-111,
IN738LC, and CM247LC). The oxidation resistance of the superalloys were evaluated by the oxidation rate
constants and the mass gains. The oxidation scales mainly consisted of outer Cr2O3 and inner Al2O3 layers at
both temperatures, as well as oxides of minor elements such as TiO2, NiCr2O4, CrTaO4, HfO2, and TaO. The
oxidation resistance of the alloys containing larger amounts of Al, W, and Ta and lower Mo and Ti concentrations
was higher than those of the other alloys. The ranking of oxidation resistance for the alloys corresponded to the
statistical prediction drawn from a response surface analysis. Furthermore, these alloys contained more Ta
oxides, such as CrTaO4 and TaO, suggesting that Ta oxides had an active role in improving the oxidation
resistance.

Keywords: alloys, oxidation, X-ray dif- ments in Ni-based superalloys are Al and Cr. They form thin
fraction, Ni-based superalloys, cyclic oxi- and continuous Al2O3 and Cr2O3 oxide layers, respectively,
dation test on the surface of the alloy. The layers glow slowly and pro-
1. INTRODUCTION vide a good diffusion barrier for additive O atoms intruding
into the underlying alloy [8-11]. Notably, Cr2O3 provides an
Ni-based superalloys have high oxidation resistance and
effective barrier up to 870 °C. Above this temperature, Cr2O3
advanced mechanical properties at high temperature. Their
becomes unstable, and then Al2O3 becomes the dominant
primary practices in high-temperature industrial applications
protective layer [8,11].
include gas turbine blades, jet engines, aerospace compo-
Alloying elements other than Al and Cr may also play
nents, and chemical plants [1-3]. Among them, gas turbine
important roles in enhancing the oxidation resistance of Ni-based
blades must work at very high temperature (over 1000 °C)
superalloys. Klein et al. [12] reported that Si and B enhance
without degradation of oxidation resistance and mechanical
the oxide layer adhesion of Co-based superalloys, while Nb
properties. To overcome this difficulty, the blades are cast as
accelerates the oxidation. Yan et al. [13] reported that Cr, Fe,
a single crystal to prevent creep and fatigue fracture in the grain
and Si in Co-based superalloys at 800 °C improved the oxidation
boundary regions, and the surface is coated with ceramic
resistance, whereas V was detrimental. They also showed that
materials to retard oxidation [2-7]. Nevertheless, the devel-
Cr changed the mechanism of oxide scale formation, and a
opment of alloys with excellent oxidation resistance and mechan-
critical amount of both Al and Cr was necessary to form a pro-
ical properties at high temperature is still required, as the above
tective oxide scale. Several reactive alloying dopants such as
schemes cannot provide perfect protection.
Hf, Zr, Y, Dy, and La improve the oxidation resistance of
The composition of a superalloy is the main factor to con-
β-NiAl by single or co-doping, as the slow outward diffusion
trol its oxidation behavior. The most important alloying ele-
of the reactive element ions inhibits the diffusion of Al ions
*Corresponding author: heejin@chosun.ac.kr [14-18].
KIM and Springer There have been divergent opinions about the effect of Ta
790 Hee-Soo Kim et al.

on the superalloy oxidation behavior [5,12,15,19,20]. Yang
[20] reported that an addition of Ta as small as 1 at% (~3.0 wt%)
improved the oxidation resistance by promoting early estab-
lishment of a protective Al2O3 layer. When 3 at% (~8.8 wt%)
of Ta was added, complex oxides such as NiMoO4, NiTa2O6,
TaO2, MAl2O4, and M2CrO4 were formed, causing degrada-
tion of the oxidation resistance. Klein et al. [12] showed that
2 at% (~5.2 wt%) of Ta weakened the oxidation resistance of
Co-based superalloys. Lu et al. [2] and Guo et al. [15] suggested
that Ta slows down the outward diffusion of Al, suppressing
the growth of oxide scales on a single-crystal Ni-based alloy
or β-NiAl. The present author [19] showed that small addi-
tions of Ta up to 5 wt% degraded the oxidation resistance at
850 °C, slowing down the formation of Al2O3 in Ni-based
superalloys. When the Ta content was greater than 5 wt%, or the
Al concentration was low, Ta enhanced the oxidation resistance
of the alloys by lowering the O activity or restraining the
outward diffusion of Al in the scale. Remarkably, the oxida-
tion rate was reduced by adding ~3–6 wt% of Ta at 1000 °C.
We developed two new Ni-based superalloys and compared
their high-temperature oxidation resistance with those of
commercial alloys such as GTD-111, IN738LC, and CM247LC.
Oxidation tests were conducted in cycle at 850 and 1000 °C.
The oxide scales were examined by X-ray diffraction (XRD)
and scanning electron microscopy (SEM) along with energy
dispersive spectroscopy (EDS) to examine the effect of alloy
composition on scale formation.
the form of bars. The specimens used in the oxidation tests were
10 mm in diameter and 3 mm in thickness. The specimen
surfaces were finished with sand papers up to #600 grit to keep
the oxidation conditions uniform for all the samples. Each
specimen was placed in an alumina crucible of 20 × 20 × 15 mm3
(length × width × height) for the oxidation tests. The crucibles
were baked for over 100 h at 1000 °C to remove humidity and
confirm that the weight remained stable in the test environ-
ment.
The oxidation tests were performed at 850 and 1000 °C. A
single cycle of oxidation was composed of the following steps.
(1) The initial specimen was put into a furnace previously
preheated at 400 °C; (2) the furnace was heated up to the target
temperature (the heating rates were 3.75 and 5 °C/min at 850
and 1000 °C, respectively); (3) static oxidation was maintained
for 15 h at the target temperature; (4) the furnace was cooled
down to ~700 °C at the rate of 1.3–2 °C/min by turning it off;

2. EXPERIMENTAL PROCEDURES

The chemical compositions of the Ni-based superalloys

investigated here are listed in Table 1. The GTD-11, IN738LC,
and CM247LC alloys are commercially available. The alloys
named as Aa1 and B1 were newly designed for this study. They Fig. 1. Schematic thermal history of a single oxidation cycle used in
were prepared by using vacuum arc melting, and then cast in this study.

Table 1. Chemical compositions of Ni-based superalloys used in this study (wt%)

Alloying elements GTD-111 IN738LC CM247LC Aa1 B1
Co 9.5 8.5 9.3 12.95 4.74
Cr 14 16 8 9.64 16.09
Mo 1.5 1.8 0.5 < 0.01 0.63
W 4 2.5 9.5 8.79 5.3
Al 3 3.5 5.5 5.14 4.87
Ti 5 3.5 0.7 0.98 1.53
Ta 3 1.5 3.2 2.93 5.98
C 0.1 0.1 0.07 0.097 0.07
B 0.01 0.01 0.15 0.016 0.017
Nb 0 1 0 0 0
Hf 0 0 1.4 < 0.01 < 0.01
Zr 0 0.06 0.01 0.007 0.007
Fe 0 0 0 0.022 0.06
Si 0 0 0 0.03 0.03
Ni Bal. Bal. Bal. Bal. Bal.
 High Temperature Oxidation Resistance of Ni-(5~13)Co-(10~16)Cr-(5~9)W-5Al-(1~1.5)Ti-(3~6)Ta Alloys 791

(5) the specimen was cooled down to ~400 °C at the rate of
2.5–3 °C/min by keeping the furnace door open; (6) the specimen
was removed from the furnace, and then (7) air cooled to room
temperature. The oxidation cycle was repeated twenty times.
A schematic thermal history of the single oxidation cycle is
shown in Fig. 1.
Between the cycles, the weight of the specimen, including
its container and the spalled scale, was measured using a pre-
cision balance to estimate the mass gain due to oxidation. After
the oxidation test, XRD was conducted to identify the phases
composing the oxide scale. Cross-sections of the oxidized
specimens were observed by using SEM with EDS.
3. RESULTS AND DISCUSSION
When a metal is oxidized, O atoms intrude into the metal,
form oxide films, and increase the mass of the matrix. The
evaluation of the mass gain occurred during the oxidation
test can be a valid criterion to examine the oxidation of the
specimen. Figure 2 shows the mass gains of the specimens during
the oxidation tests at 850 and 1000 °C. For all specimens, the
weights increased with time by oxidation. Notably, the square
of the mass gain (Δm) per unit area is proportional to time
2 2 2
(t): Δm = kpt where kp (mg /cm ·s) is the oxidation rate con-
stant, which is related to the diffusion of cations or anions across
the oxide layer [21,22]. In this study, every cycle had an
identical thermal history for a designated target temperature,
and the thermal histories at 850 and 1000 °C had identical
time durations at the oxidation temperatures. Therefore, a sin-
gle cycle of the oxidation test may be considered as a time
unit: Δm2 = kcnc where kc (mg2/cm2·cycle) is the oxidation rate
2
constant and nc is the number of cycles. The plots of Δm as a
function of the cycle at each temperature are shown in Fig. 3. The
symbols represent the experimental data, whereas the solid
lines behind the symbols indicate the best-fitted lines. The fig-
ure shows that the experimental results followed very well the

Fig. 2. Mass gains during oxidation tests of the Ni-based superalloys, as functions of the cycle at (a) 850 °C and (b) 1000 °C.

Fig. 3. Plots of squares of the mass gains as functions of the cycle at (a) 850 °C and (b) 1000 °C. The symbols indicate the experimental results,
while the solid straight lines represent the best-fitted lines.
792 Hee-Soo Kim et al.
Fig. 4. Variation of oxidation rate constants, kc, with oxidation tem-
perature for the Ni-based superalloys tested in this study.
aforementioned kinetic equation. The slopes of the best-fitted
lines indicate the oxidation rate constants kc. These constants,
plotted at the oxidation temperatures for all the alloys inves-
tigated in this study, are shown in Fig. 4.
After 20 cycles of oxidation, the weights of the specimens
2
increased approximately from 0.14171 to 0.63265 mg/cm at
2
850 °C, and from 0.34988 to 4.11673 mg/cm at 1000 °C, as
shown in Fig. 2. These mass gains corresponded to oxidation
−4 −2
rate constants ranging between 2.058 × 10 and 1.979 × 10
2 −4
mg/cm ·cycle at 850 °C, and between 4.955 × 10 and 8.495 ×
−1 2
10 mg/cm ·cycle at 1000 °C, as shown in Fig. 4. The oxidation
rates of CM247LC, Aa1, and B1 did not show substantial
Fig. 5. Scanning electron microscopy images of (a) GTD-111, (b) IN738LC, (c) CM247LC, (d) Aa1, and (e) B1 alloys.
differences between 850 and 1000 °C, although they slightly
increased with the temperature. The oxidations of GTD11 and
IN738LC were severe at 1000 °C, compared with those at
850 °C. At 850 °C, B1 showed the best oxidation resistance.
Its oxidation rate was lower than that of CM247LC, which
had the lowest oxidation rate among all the commercial alloys
investigated in this study. The oxidation rate of Aa1 was between
those of CM247LC and IN738LC. At 1000 °C, Aa1 exhibited
the best oxidation resistance, while B1 showed a good oxidation
resistance similar to that of Aa1.
The alloys with a low oxidation rate were characterized by
compositions comprising low quantities of Mo and Ti and high
amounts of Al, W, and Ta, compared with the other alloys, at
both temperatures. The alloys with high Cr concentration showed
excellent or good resistance to oxidation at 850 °C, but their
oxidation rates increased severely at 1000 °C, as Cr oxide
becomes volatile at temperatures higher than ~900 °C. The
microstructure also can affect the oxidation rate by promote
or inhibit diffusion, generally. However, the microstructure does
not seem to have meaningful influence on the oxidation rate
in this study because the alloys does not show remarkable
difference in the microstructure, as shown in Fig. 5, showing
very high density of γ’ precipitations with the size about 0.3
~ 0.5 μm. Therefore, the oxidation rate of the alloys are con-
sidered to be determined predominantly by the composition
in this work.
The results of this work are in good agreement with the
statistical study reported by Park et al. [19,23]. Their report
suggested that Mo and Ti promote oxidation, while Al and Ta
significantly decrease the oxidation rate of Ni-based superal-
loys. Mo is harmful to oxidation resistance [24,29] owing to
 High Temperature Oxidation Resistance of Ni-(5~13)Co-(10~16)Cr-(5~9)W-5Al-(1~1.5)Ti-(3~6)Ta Alloys
the volatility of its oxide; besides, Mo inhibits the formation
of Cr2O3 and promotes oxide spallation [26,27]. Previous works
showed that TiO2 is typically found in alloys with high oxida-
tion rates [19,23]. Sato et al. [32] thermodynamically calcu-
lated the defect chemistry of oxide scales, and suggested that
the addition of Al and Cr facilitates the formation of a con-
tinuous Al2O3 layer, whereas W, Ta, Ti, and Mo inhibit it. In
addition, other researchers have proposed that Ta retards the
growth of Al by reducing the O activity [32,33] as well as
simultaneously suppressing the Al outward diffusion [4,15]
and O inward diffusion [32]. These reports imply that Ta may
be detrimental to oxidation resistance because it impairs the
formation of a highly protective Al2O3 layer. However, Ta can
improve the oxidation resistance by retarding the diffusion
processes required for the oxidation to occur. In practice, the
effect of Ta on the oxidation rate seems to change depending
on the oxidation temperature and concentrations of Al and Ta,
which determine the possibility to form a continuous Al2O3
layer [19]. W and Ti might have similar roles to Ta in oxidation.
Park et al. [23,34] reported the regression coefficients for
the mass gain of Ni-based superalloys after 20 cycles of oxidation
in terms of the main alloying elements by using the response
surface analysis for the effects of Co (~0–15 wt%), Cr (~8–
15 wt%), Mo (~0–5 wt%), W (~0–10 wt%), Al (~3–8 wt%), Ti
(~0–5 wt%), and Ta (~0–10 wt%). According to their work, Al,
W, Cr, and Ta reduced the mass gain of the alloy at 850 °C.
At 1000 °C, Al, W, Co, and Ta improved the oxidation resis-
tance, while Cr and Ti had a detrimental effect. Figure 6 shows
the mass gains from the present work and the calculation for
the compositions of the alloys in this study. Although there
were some differences between the present results and the
estimated values, the overall oxidation tendencies were similar.
The differences between the two sets of data may be caused
by several reasons. The concentration of some alloying ele-
Fig. 6. Comparison of mass gains after 20 cycles of oxidation at (a) 850 °C and (b) 1000 °C with the data estimated by response surface analysis.
The line segments between the data points were drawn for ease of comparison.
793
ments, i.e., Cr in GTD-111, IN738LC, and B1, was close to, or
even above, the concentration boundaries of the response
surface analysis. Park et al. [23,34] used the Box-Behnken
scheme for the response surface analysis to minimize the
number of experimental runs; however, this might cause inac-
curate results near the marginal values of the variables. Fur-
thermore, IN738LC and CM247LC included Nb or Hf, which
were not considered in Park’s model, although researchers have
reported that minor elements such as Nb and Hf have a con-
siderable importance in oxidation resistance [13,18]. The
specimen microstructures may also have an impact; con-
versely to the model alloys used in Park’s previous work, the
alloys used in this study were directionally solidified.
Note that Aa1 alloy exhibited a decreased oxidation rate
constant value measured at 1000 °C in comparison with that
of 850 °C. Aa1 has much a higher Co content than the other
alloys studied in this work. Park et al. [34] showed that Co
has little effect on the oxidation resistance of the superalloy
at 850 °C but seemed to improve the oxidation resistance at
1000 °C, especially when it was added more than 7.5 wt%.
Therefore Aa1 can be protected by the presence of Co more
effectively at 1000 °C that it is at 850 °C.
The XRD spectra of the oxidized layers of the alloys are
shown in Fig. 7. Various types of oxides were formed during
the oxidation tests. At both temperatures of 850 and 1000 °C,
the spectra included peaks of NiO, Ni3Al, Al2O3, NiCr2O4,
Cr2O3, CrTaO4, and TiO2. At 1000 °C, GTD-111 exhibited more
peaks of Cr2O3 and TiO2 than any other alloy.
Figure 8 shows the cross-sectional SEM images of the
alloys after 20 cycles of oxidation at 850 °C. Notably, the oxide
scales consisted of Cr oxide layers, such as Cr2O3 and NiCr2O4,
near the surface, and Al2O3 layers underneath the Cr oxide
layers. For most alloys, Al2O3 was in the form of discontinu-
ous agglomerates elongated in a direction perpendicular to
794 Hee-Soo Kim et al.

Fig. 7. X-ray diffraction spectra of Ni-based superalloys after 20 cycles of oxidation at (a) 850 °C and (b) 1000 °C.

Fig. 8. Cross-sectional scanning electron microscopy images of (a) GTD-111, (b) IN738LC, (c) CM247LC, (d) Aa1, and (e) B1 alloys after 20
cycles of oxidation at 850 °C.

the surface. In the case of Aa1, a partially continuous Al2O3
layer was also found. GTD-111 exhibited a TiO2 layer near the
surface, while CM247LC had some NiO. CrTaO4 was found
in the depths, similar to NiCr2O4, in CM247LC, Aa1, and B1,
which exhibited slower oxidation rates than the other alloys,
as shown in Figs. 2 and 3. Probably, CrTaO4 enhanced the
oxidation resistance of the alloys.
Figures 9 and 10 show the cross-sectional SEM images of
the alloys after 20 cycles of oxidation at 1000 °C. The overall
cross-sectional structures were analogous to those observed
for the samples oxidized at 850 °C. The Al2O3 layer was con-
tinuous, except in the case of GTD-111. Traces of HfO2 (in
CM247LC) and TaO (in Aa1) were also found. A discontin-
uous Al2O3 layer may have been the cause of the high oxida-
tion rate of GTD-111. In the case of IN738LC, Al2O3 existed
as a thin layer or was in a mixed form with Cr2O3. The alloys
with a continuous Al2O3 layer, i.e., CM247LC, Aa1, and B1,
exhibited lower oxidation rates, as shown in Figs. 2–4.
Giggins and Pettit [35] suggested the oxidation mechanism
of Ni-Cr-Al alloys as follows. The first oxide layer on the sur-
face of the alloy is predominantly made of Ni(Cr,Al)2O4 and
NiO. The formation of Cr2O3 and Al2O3 is controlled by the
diffusion of Cr, Al, and O. As the activity of O required to
oxidize Cr is smaller than that required for Ni(Cr,Al)2O4 and
 High Temperature Oxidation Resistance of Ni-(5~13)Co-(10~16)Cr-(5~9)W-5Al-(1~1.5)Ti-(3~6)Ta Alloys 795

Fig. 9. Cross-sectional scanning electron microscopy images of (a) GTD-111, (b) IN738LC, and (c) B1 alloys after 20 cycles of oxidation at 1000 °C.

Fig. 10. Cross-sectional scanning electron microscopy images of (a, b) CM247LC and (c, d) Aa1 alloys after 20 cycles of oxidation at 1000 °C.

NiO, O diffuses into the matrix and form Cr2O3 below the
surface layer. Moreover, the O activity to form Al2O3 is even
smaller than that for Cr2O3, and Al2O3 precipitates beneath
Cr2O3. For all alloys in this study, Cr2O3 was found near the
surface, and Al2O3 existed below the Cr2O3 layer at both 850
and 1000 °C, as shown in Figs. 8–10. However, NiCr2O4
appeared on the surface, although only in CM247LC and Aa1
at 1000 °C. NiO was found in CM247LC and Aa1 at 850 °C
only. In all other cases, a little amount of NiO or NiCr2O4 was
found as a mixed form between the Cr2O3 and Al2O3 layers.
Most of NiO seemed to be spalled off during the oxidation
test, owing to the stress arisen from the large mismatch between
the thermal expansion coefficients of NiO and Cr2O3, which
was formed just underneath the NiO layer [36].
TiO2 is known to typically form a layer on the surface [4,37,38].
In this study, TiO2 was found in GTD-111, and a mixture of
Cr2O3 and TiO2 existed in B1 at 1000 °C, although all the alloys
used in this work had Ti as an alloying element. Seal et al. [38]
reported that TiO2 did not form on the surface after a short-time
oxidation (~10 h) at 900 °C, possibly owing to its low activity
in the IN-738LC alloy, compared with that of Cr and Ni. A long
time, over 100 h, was necessary to form TiO2. Similarly, in this
study, TiO2 was expected to form after more cycles of oxidation
also in alloys other than GTD-111 and B1.
In CM247LC, Aa1, and B1, Ta oxides such as CrTaO4 and
TaO were observed. Although GTD-111 and IN738LC had Ta
as an alloying element, no Ta oxide was found. GTD-111 and
IN738LC had a higher Ti content than the other alloys. Ti likely
impeded the formation of Ta oxides. This was consistent with
the fact that Ti weakens the effect of Ta at 850 °C, as previously
796 Hee-Soo Kim et al.
suggested by the response surface analysis [23,34]. As the
oxidation of GTD-111 and IN738LC became severe at 1000 °C,
Ta oxides likely played a great role in improving the oxida-
tion resistance of the alloys. Park et al. [23] reported that the
effect of Ta addition on oxidation resistance was clearer at
1000 °C than at 850 °C. Guo et al. [15] pointed out that Ta atoms
are large, and thus their diffusion is slow. Ta oxides may form
more easily at 1000 °C than at 850 °C, likely enhancing the
oxidation resistance of the alloys at 1000 °C.
4. CONCLUSIONS
The oxidation resistance of Ni-based superalloys was eval-
uated by cyclic oxidation tests at 850 and 1000 °C. The alloys
used in this study included the commercially available GTD-111,
IN738LC, and CM247LC alloys. Two newly designed superal-
loys were also investigated. The oxidation scales mainly con-
sisted of outer Cr2O3 and inner Al2O3 layers at both 850 and
1000 °C. The oxidation of GTD-111 and IN738LC became
severe at 1000 °C; the two alloys did not contain Ta oxides
after the tests. Presumably, Ta oxides improved the oxidation
resistance of the other alloys. The ranking of oxidation resis-
tance for the superalloys corresponded to the statistical predic-
tion drawn from a response surface analysis, suggesting that
the presence of Al, W, Co, and Ta remarkably improved the
oxidation resistance.
ACKNOWLEDGEMENTS
This work was supported by a grant from the Fundamental
R&D Program for Core Technology of Materials (10041233)
funded by the Ministry of Trade, Industry and Energy of the
Republic of Korea.
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