ISIJ International, Vol.

56 (2016),
ISIJ International,
No. 2 Vol. 56 (2016), No. 2, pp. 319–325

Microstructure Control of Dual-Phase Steels through Hot-Dip

Al–Mg–Si Alloy Coating Process

Naoki TAKATA,1)* Tadashi TSUKAHARA,2) Satoru KOBAYASHI3) and Masao TAKEYAMA3)

1) Formerly Department of Metallurgy and Ceramics Science, Graduate School of Science and Engineering, Tokyo Institute of
Technology. Now at Department of Materials Science and Engineering, Nagoya University, Furo-cho, Chigusa-ku, Nagoya,
463-8303 Japan. 2) Formerly Graduate Student, Graduate School of Science and Engineering, Tokyo Institute of Tech-
nology. Now at NHK Spring Co., Ltd., 3-10 Fukuura, Kanazawa-ku, Yokohama, 236-0004 Japan.
3) Department of Metallurgy and Ceramics Science, Graduate School of Science and Engineering, Tokyo Institute of Technol-
ogy, 2-12-1-S8-8, Ookayama, Meguro-ku, Tokyo, 152-8552 Japan.
(Received on July 24, 2015; accepted on November 2, 2015)

This study investigates the γ→α transformation kinetics of Fe–Mn–C dual-phase steels at a temperature
above the melting point of an Al–8.2Mg–4.8Si (wt.%) alloy coating formed on their surface by hot-dipping
process. Using an experimentally determined time-temperature-transformation (TTT) diagram for a model
steel of Fe–1.5Mn–0.1C (wt.%), the volume fraction of martensite is controlled through the intercritical
heat treatment incorporated into the hot-dipping process. The microstructural observations confirm that
this combined process route makes it possible to fabricate hot-dipped Al alloy-coated dual-phase steels
with a controlled microstructure.

KEY WORDS: aluminizing; galvanizing; time-temperature-transformation (TTT) diagram; transformation

kinetics; Fe–Al intermetallics.

of an Al–Mg–Si alloy coating and the time-temperature-

1. Introduction
transformation (TTT) diagram for a plain low-carbon steel
The potential for Zn prices to increase due to limited are shown in Fig. 1(a), together with the corresponding
resources of the metal has created a need to develop alter- microstructures illustrated in Figs. 1(b)–1(e). In this process,
natives to galvanizing steel such as a hot-dipped Al–Mg–Si the ferrite (α) in the steel sheet transforms to austenite (γ)
alloy coating. Tsuru et al.1–5) have found that an Al–8.2Mg– by heating to the reduction temperature corresponding to a
4.8Si (wt.%) alloy coating with a fine eutectic microstructure single γ phase (or γ + α two phase) region (Fig. 1(b)). After
of α-Al and Mg2Si produces a sufficient sacrificial anodic holding at the reduction temperature, the steel sheet is then
effect, with hydrogen entry and embrittlement being a much cooled to a dipping temperature above the melting point of
lower risk than with galvanized steel.4,5) This hot-dipping the Al alloy coating. During this cooling period, the α phase
Al–Mg–Si alloy coating process is therefore expected to nucleates on grain boundaries in the γ matrix, resulting in a
increase automotive applications of high strength steels with two-phase microstructure of γ and α phases at the dipping
a dual-phase microstructure of martensite and ferrite by temperature (Fig. 1(c)). Following hot-dipping of the steel
effectively replacing galvanized high strength steel sheet.6,7) sheet in a molten Al alloy bath, Fe–Al intermetallic layers
However, such application requires an ability to control
the steel microstructure through the hot-dipping coating
process, as well as control the formation and growth of
Fe–Al intermetallic layers at the interface between the steel
substrate and Al alloy coating.8–10)
Conventional continuous hot-dipping galvanizing pro-
cess6) involves heating steel sheet/strip to around 800°C
in a N2/H2 reducing atmosphere prior to immersion in a
Zn bath.11–16) However, for this same process to be applied
to the fabrication of an Al alloy coating dual-phase steels,
it is necessary to control the steel microstructure through
a sequence of heating and cooling during the hot-dipping
process. A representative heat profile for the hot-dipping
Fig. 1. (a) Thermal profile of a steel sheet during hot-dipping pro-
cess, together with its time-temperature-transformation
* Corresponding author: E-mail: takata@numse.nagoya-u.ac.jp (TTT) diagram and (b–e) corresponding microstructures
DOI: http://dx.doi.org/10.2355/isijinternational.ISIJINT-2015-441 during hot-dipping.

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 ISIJ International, Vol. 56 (2016), No. 2

are formed at the interface between the steel and molten

Al alloy (Fig. 1(d)). The steel sheet is then rapidly cooled
by gas wiping to control the coating thickness11,14) and an
additional forced air cooling,6) which causes any remaining
γ phase to transform to martensite. This produces a final
dual-phase microstructure of ferrite and martensite (α + α’)
(Fig. 1(e)). In the conventional process, γ + α two phase
microstructure often changes during the cooling and hot-
dipping processes after the reduction treatment, whereby it
would be difficult to control both the steel microstructure
(γ + α two phase microstructure) and the interface micro-
structure between the steel sheet and liquid Al alloy (Fe–Al
intermetallic layers) all together. One of the potential routes
to control both microstructures independently is the con-
trolled cooling process or the additional heating (and hold-
ing) process above the dipping temperature (to control γ +
α two phase microstructure) prior to the hot-dipping process
(to control the Fe–Al intermetallic layers). Thus, making
control over the kinetics of the γ→α transformation is one
of most important issues to achieve these processes for the
fabrication of Al alloy-coated dual-phase steels.
This study investigates the kinetics of the γ→α trans-
formation that occurs in a model dual-phase steel with
Fe–Mn–C ternary compositions. Based on the experimen-
tally determined time-temperature-transformation (TTT)
diagram, an attempt has been made to fabricate the Al–Mg– Fig. 2. Chemical compositions of the steels studied plotted on (a)
Si alloy-coated dual-phase steels. These results are herein Fe–Mn binary phase diagram and (b) 0.1 at.% C vertical
section of the Fe–Mn–C ternary phase diagram.
discussed in terms of developing an appropriate sequence
of heat treatment to control the microstructure of Al–Mg–
Si alloy-coated dual-phase steels during the hot-dipping
process. air in the glove box was fully replaced with the reducing
Ar–H2 gas using the equipped gas inlet and purge systems
(Fig. 3(b)). In order to cut off the ambient air supply dur-
2. Experimental Procedure
ing these experiments, the inside of the glove box was kept
The chemical compositions of the steels used in this in a constant positive pressure of approximately 2 × 104
study were Fe–(1.5, 3.5)Mn and Fe–(1.5, 3.5)Mn–0.1C (all Pa by controlling the gas purge flow rate. This reducing
compositions are given in weight percent unless specified atmosphere served to prevent oxidation of the sample sur-
otherwise). These compositions were plotted on a Fe–Mn face makes it possible to achieve the defect-free Al alloy
binary system and a 0.1% C section of the Fe–Mn–C ternary coatings, as shown in Fig. 3(d). The container for these two
system was prepared using the thermodynamic database of furnaces was cooled by flowing water (Fig. 3(a)). To deter-
PanIron17) (Fig. 2). For each steel composition, 50 kg ingots mine the γ→α transformation temperature under continuous
were prepared by vacuum melting and casting, which were cooling, each of the steel types was heated (austenitized)
homogenized at 1 200°C for 7.2 ks and then hot-rolled to at 900°C for 600 s, and then cooled under the reducing
plates with a thickness of approximately 30 mm. These atmosphere inside the glove box. To prepare a time-
plates were held at 1 230°C for 7.2 ks, hot-rolled to sheets temperature-transformation (TTT) diagram, the samples
with a thickness of approximately 4 mm, and then cold- were austenitized at 900°C for 600 s, and then quenched
rolled to 1 mm in thickness. Pieces cut from these cold- in a bath of molten Al alloy at temperatures ranging from
rolled sheets were mechanically polished with #800 emery 650 to 780°C for 2–1 800 s, followed by a water quench.
paper, and then hot-dipped in molten Al–8.2Mg–4.8Si The heat profiles were measured by K-type thermo-couples
(wt.%) alloy saturated with Fe. The method used to prepare welded on the sample surface. Examples of the heat profiles
this Fe-saturated Al–Mg–Si alloy has been described else- obtained by hot-dipping in the molten Al alloy (within the
where.9,18) glove box) for 10 s at temperatures of 650, 700, and 750°C
Hot-dipping experiments were carried out under a reduc- are provided in Fig. 4. Upon immersion, the sample tem-
ing atmosphere using the customized glove box system, perature rapidly decreased from 900°C (i.e. within 5 s) to
which as shown in Fig. 3. This system contains both a the temperature of the Al alloy melt.
reducing furnace and Al alloy bath furnace (Figs. 3(b), 3(c)) Trial fabrication of Al alloy-coated dual-phase steel
so as to allow pre-heating (austenitizing) and hot-dipping sheets was carried out using an Rhesca hot-dip process
to be performed under an Ar-3vol.%H2 gas atmosphere at a simulator.11,19) The steel sheets with a dimension of
constant gas flow rate of 3.3 × 10 − 5 m3/s (2.0 l/min) with 150 mm × 50 mm × 1 mm were heated to 900°C for 600 s,
a controlled dew point of approximately − 20°C. Note that, and then cooled down to 750°C under an Ar-5 vol.% H2
before the heating or hot-dipping experiments, the ambient atmosphere with a dew point set to approximately − 30°C,

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Fig. 3. Customized glove box system used in this study: (a) schematic, (b) appearance, (c) two furnaces in the storage
box cooled by flowing water, (d) appearance of samples prepared using the system.

Fig. 4. Representative thermal profiles of steel samples hot-

dipped in Al alloy melt at different temperatures to pro- Fig. 5. Cooling profiles of Fe–Mn–C steel samples after austen-
duce a TTT diagram. itizing at 900°C.

followed by holding at 750°C for 600 s. After that, these

sheets were hot-dipped in molten Al alloy at 670°C for
different lengths of time, followed by rapid cooling by gas
wiping. These heat profiles of the sheets were measured
using K-type thermo-couples welded on the sheet surface.
The precise heat profile experimentally measured will be
described in further detail later.
The microstructure of the prepared samples was observed
by optical microscopy. The observed sample surfaces were
mechanically polished and etched with a 3% Nital solu-
tion. The sample surface ion-polished by a cross section
polisher at 5 kV for over 36 ks was observed by a scanning
electron microscope (SEM) operating at 15 kV. In order to
evaluate the volume fraction of α phase in microstructures
of the samples, the average area fractions of α phase were
measured using five optical micrographs for one sample. A
series of optical micrographs for the present measurement
were taken at a fixed magnification of × 500.
3. Results and Discussion
3.1. Continuous-Cooling-Transformation Diagram of
Fe–Mn–C Steels
Figure 5 shows the temperature profiles of the Fe–Mn–C
steel samples during the air-cooling after austenitizing pre-
treatment at 900°C for 600 s. These profiles show that the
temperatures decreases at a rate of approximately 15°C/s
above 800°C for all samples. There is a noticeable differ-
ence in the cooling profiles below 800°C. In the case of the
Fe–1.5 Mn sample, the rate of cooling slows at 770°C and
the temperature remains stable for a few seconds, followed
by a period of cooling at a constant rate of approximately
10°C/s to below 500°C. This reduction in the rate of cooling
is caused by the exothermal reaction of γ→α transformation,
and can also be seen with the profiles of the Fe–3.5Mn and
Fe–1.5Mn–0.1C samples at 640°C and 740°C, respectively.
However, no change in slope was observed with the Fe–
3.5Mn–0.1C sample.

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The temperatures at which γ→α transformation was hot-dipped at 650°C, a number of α grains are also formed
observed to start in Fig. 5 were plotted together with the A3 along the prior austenite grain boundaries after 2 s (Fig.
temperatures from the phase diagrams (Fig. 2) to prepare the 8(c)), but these grow much faster at 650°C to occupy more
continuous-cooling-transformation (CCT) diagram of Fe– than 90% in volume fraction after 600 s (Fig. 8(d)). A few
1.5Mn, Fe–3.5Mn and Fe–1.5Mn–0.1C steels. This result grains of lamellar pearlite were locally observed after 600 s.
is shown in Fig. 6. This demonstrates that the addition of Figure 9 shows the change in the volume fraction of
0.1%C to a Fe–1.5 Mn alloy makes the γ→α transforma- ferrite (α phase) with dipping time at various temperatures.
tion sluggish, with the addition of 2% Mn also retarding The volume fraction increases with increasing time. It
the transformation kinetics by an order of magnitude. This reaches to 73% after 600 s at 750°C, which corresponds to
importantly shows that the present steels would allow the the equilibrium volume fraction of α phase calculated using
two-phase microstructure of γ and α phases to be controlled the thermodynamic database of PanFe.17) In the samples
in a cooling rate ranging from 10 to 100°C/s, which cor- held at 700°C, the average volume fraction of the α phase
responds to the initial air-cooling period of the continuous is 13% after 2 s, and then increases with time to a value of
hot-dipping coating process.6,7) 80% at 600 s that is comparable to the equilibrium volume
fraction of 83%. In the samples held at 650°C, the volume
3.2. Time-Temperature-Transformation Diagram of fraction of the α phase rapidly increases to become almost
Fe–1.5Mn–0.1C Steel saturated at 93% after 600 s, which is also equivalent to
As was discussed in the previous section 3.1, the γ→α its equilibrium volume fraction (95%). These results dem-
transformation kinetics of Fe–1.5Mn–0.1C steel is favor-
able for controlling the two-phase microstructure of γ and
α phases during air-cooling, so that this composition was
selected as a model case for the dual-phase steel. In order to
experimentally determine the time-temperature-transforma-
tion (TTT) diagram for this steel, the microstructure of sheet
samples was observed after being hot-dipped in Al alloy at
various temperatures. Figure 7 presents optical micrographs
showing the microstructure produced by hot-dipping at
750°C for various times (followed by water quenching).
The fully martensitic structure (α’) was observed in the
sample hot-dipped for 2 s (Fig. 7(a)) indicating that a single
γ-phase microstructure was maintained at 750°C. Increasing
the dipping time to 10 s produced a number of elongated
ferrite (α) grains with a mean width of approximately 5 μm
along the prior austenite grain boundaries in the martensite
structure (Fig. 7(b)), which indicates that the α grains grow
by consuming the γ phase at 750°C. The volume fraction of
this α phase increases with dipping time to approximately
Fig. 7. Optical micrographs of Fe–1.5Mn–0.1C steel dipped in
70% of the sample after 600 s (Figs. 7(c), 7(d)). molten Al alloy at 750°C for (a) 2, (b) 10, (c) 60 and (d)
Figure 8 shows optical micrographs of steel samples hot- 600 s. All samples were austenitized at 900°C for 600 s.
dipped at 700 and 650°C for different times (followed by
water quenching). The samples hot-dipped at 700°C contain
the granular α grains on prior austenite grain boundaries
even after 2 s (Fig. 8(a)). These α grains grow to approxi-
mately 10 μm in size after 600 s (Fig. 8(b)). In the sample

Fig. 8. Optical micrographs of Fe–1.5Mn–0.1C steel dipped in

molten Al alloy at (a, b) 700 and (c, d) 650°C for (a, c) 2
Fig. 6. Continuous-cooling-transformation (CCT) diagram of and (b, d) 600 s. All samples were austenitized at 900°C
γ→α transformation in Fe–Mn–C steels. for 600 s.

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 ISIJ International, Vol. 56 (2016), No. 2
onstrate the slower γ→α transformation kinetics at higher
temperature within a temperature range from 750 to 650°C.
Figure 10 shows the time-temperature-transformation
(TTT) diagram for Fe–1.5Mn–0.1C steel determined in this
study. In this figure, the numbers beneath the various sym-
bols represent the volume fraction of the α phase. The dia-
gram shows how the γ→α transformation starts in less than
20 s at temperatures between 650 to 750°C (Fs). The point
at which γ→α transformation finishes (Ff) can be deduced
from the change in the volume fraction of α phase with time
(Fig. 9), creating a line located above 300 s, which shows
the transformation time is reduced at lower temperature at
least within a temperature range from 750 to 650°C. Note
that the localized pearlite structure in the sample hot-dipped
at 650°C for 600 s (Fig. 8(d)) also gives a pearlite transfor-
mation start line (Ps).
3.3. Fabrication of Hot-Dipped Al–Mg–Si Alloy Coated
Dual-Phase Steels
In order to fabricate hot-dipped Al alloy-coated dual-
phase steel with a volume fraction of martensite of ~30%,
Fe–1.5Mn–0.1C steel sheets were austenitized at 900°C for
600 s, and then cooled down to 750°C (at a cooling rate
of approximately 7°C/s), followed by holding for 600 s to
equilibrate in the two-phase region of α and γ phases. Sub-
sequently, the sheets were hot-dipped in Al alloy at 670°C,
and then rapidly cooled by gas wiping. The measured
Fig. 9. Change in the volume fraction of ferrite in Fe–1.5Mn–
0.1C steel with dipping time in the molten Al alloy at dif-
ferent temperatures.
Fig. 10. Time-temperature-transformation (TTT) diagram of Fe–
1.5Mn–0.1C steel. The numbers beneath the symbols
represent the volume fraction of ferrite.
323
cooling rate of the steel surface till 400°C (the martensite
start temperature of this steel is approximately 450°C20,21))
was approximately 25°C/s, which suggests that the γ phase
would transform to martensite during the rapid cooling. A
representative heat profile for this is plotted on the TTT
diagram in Fig. 11, which shows how well the temperature
was controlled by the cooling/heating system of the hot-
dipping process simulator used. The photographs in Fig. 12
also show that the steel sheets were uniformly coated with
Al alloy without any discernible defects, regardless of the
hot-dipping time. The dark areas on the coating surface are
an oxide film believed to be from the surface of the molten
Al alloy.
Figure 13 presents the optical micrographs showing the
steel microstructure and the interface between the steel sheet
and the Al alloy coating in the prepared sample. These opti-
cal micrographs illustrates the dual-phase microstructure of
fine martensite (α’) grains distributed in an equiaxed ferrite
(α) microstructure with a mean grain size of approximately
15 μm (Figs. 13(a), 13(b)). Most of the martensite grains
are equiaxed, whereas some interconnect to form an irregu-
lar shape that is seen in the sample hot-dipped after 2 and
Fig. 11. Thermal profile of the heat treatment process with the
aim of fabricating the Al alloy coated dual-phase steel
with 30% volume fraction of martensite (austenitizing at
900°C for 60 s → cooling → holding at 750°C for 600 s
→ hot-dipping at 670°C → rapid cooling).
Fig. 12. Appearance of Al alloy-coated steels prepared using a
hot-dip process simulator.
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 ISIJ International, Vol. 56 (2016), No. 2
Fig. 13. Optical micrographs showing the microstructure of (a, b)
dual-phase steel and (c, d) the interface between this
sheet and an Al alloy coating produced by hot dipping at
670°C for (a, c) 2 s and (b, d) 100 s.
Fig. 14. Backscattered electron image showing the Fe–Al alloy
layer of an Al alloy-coated dual-phase steel (dipped at
670°C for 2 s).
100 s. The minute observation revealed the fine substruc-
tures in these martensite grains, corresponding to the packet
or block structures. The volume fraction of martensite is
approximately 26% in all samples. These results indicate
that there is scarcely any change in the α and γ two-phase
microstructure during hot-dipping at 670°C. At the interface
between the Al alloy coating and steel substrate, a Fe–Al
alloy layer with a mean thickness of 6 μm is formed after
2 s of hot-dipping (Fig. 13(c)), which grows to a thick-
ness of 20 μm after 100 s (Fig. 13(d)). A back-scattered
electron image of the Fe–Al alloy layer in the sample hot-
dipped for 2 s is shown in Fig. 14. This indicates a dual
layer structure of θ-FeAl3 phase on the Al alloy coating
and a thick η-Fe2Al5 phase layer on the steel substrate.
The structure corresponds well to that formed on pure iron
sheet hot-dipped in Al–Mg–Si alloy at 750°C (followed by
water quenching),9) whereas the layer thickness is somewhat
smaller than that in the sample hot-dipped at 750°C, which
is likely due to lower hot-dipping temperature in the present
study. Note that the η phase layer has a relatively uniform
interface with the dual-phase steel substrate, which suggests
the steel microstructure has a slight effect on the growth of
the η phase into the steel substrate.
Based on the results presented thus far, a proposed
process concept to control the microstructure of dual-
© 2016 ISIJ
Fig. 15. Proposed heat treatment process for the microstructural
control of hot-dipped Al alloy-coated dual-phase steels.
phase steels during hot-dipping with an Al alloy coating
is presented in Fig. 15. This is a two-step heat treatment/
hot-dipping approach, whereby steel sheets are first aus-
tenitized under a reducing atmosphere, and then cooled to
an intercritical temperature between A1 and A3 in order to
equilibrate in a two-phase region of α and γ phases (the
heat profile needs to pass the γ→α transformation finish line
(Ff) in the TTT diagram). This allows the volume fraction
of the α phase to be controlled by changing the holding
temperature, after which the steel sheets are immediately
hot-dipped in Al alloy and rapidly cooled to transform the
γ phase to martensite and create a dual-phase microstruc-
ture. The thickness of the Fe–Al alloy layer formed at the
interface between the Al coating and steel substrate can, if
needed, be controlled by changing the dipping time (or dip-
ping temperature). It should also be noted here that reducing
the difference between the intercritical holding temperature
and dipping temperature can prevent any change in the
steel microstructure during hot-dipping, as this temperature
difference provides the undercooling to provide the driving
force for the γ→α transformation. In order to minimize
the amount of undercooling at the dipping temperature, a
two-phase region of α and γ phases can also be controlled
through the addition of alloying elements in terms of ferrite
or austenite stabilizers. The addition of alloying elements
can also change the γ→α transformation kinetics to provide
greater control over the two-phase microstructure of α and γ
phases through the intercritical heat treatments. In addition,
considering the industrial continuous hot-dipping coating
line,6) it could be required to achieve the austenitizing and
intercritical treatments at lower temperature for shorter time.
In order to solve these issues, optimizing the alloying ele-
ments is needed to control two kinetics of α→γ and γ→α
transformations as well. Thus, further alloy modification is
desirable, especially when it comes to controlling the multi-
phase microstructures of advanced high strength steels such
as TRIP and TWIP22) through a combination of heat treat-
ment and hot-dipping.
From an engineering point of view, the adhesiveness of
the Al alloy coating layer on the dual-phase steel sheet is an
important consideration with advanced high strength steels.
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The present process can control the layer thickness of the
Fe–Al intermetallic phase on the dual-phase steels with
various volume fraction of martensite. This awaits future
work in order to understand that the martensite in the α
matrix plays a role in the delamination behavior of the Al
alloy coating.
4. Summary
This study has identified the γ→α transformation kinet-
ics of Fe–Mn–C steels at a temperature above the melting
point of an Al–Mg–Si alloy used for hot-dip coating. From
experimentally determined CCT and TTT diagrams, hot-
dipped Al–Mg–Si alloy-coated dual-phase Fe–1.5Mn–0.1C
steel sheets with a controlled volume fraction of martensite
have been successfully fabricated by combining a suitable
heat treatment with the hot-dipping process. This entails
first equilibrating the steel at an intercritical temperature in
the α + γ two-phase region to control the volume fraction of
α-Fe, with rapid cooling after the hot-dipping being used to
transform the γ phase to martensite and create the required
dual-phase microstructure. Microstructural observations
have confirmed that this processing route is effective for
coating dual-phase steels with Al alloy by hot-dipping
process.
Acknowledgments
The support of the Ministry of Education, Sports, Culture,
Science, and Technology of Japan through the Element Sci-
ence Technology Project “Development of Hot-Dipped Alu-
minum Alloy Coated Steels” is gratefully acknowledged.
325
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