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Effects of precipitation on the scale and grain growth in 9% Cr tempered

martensite steel upon steam oxidation

Article in Materials Characterization · July 2020

DOI: 10.1016/j.matchar.2020.110497

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Materials Characterization
journal homepage: http://ees.elsevier.com

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Effects of precipitation on the scale and grain growth in 9% Cr tempered martensite
steel upon steam oxidation
Houyu Ma a ,1 , Yinsheng He b ,1 , Yue Liu a ,⁎ , Keesam Shin c ,⁎

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a
State Key Lab of Metal Matrix Composites, School of Materials Science and Engineering, Shanghai Jiao Tong University, Shanghai 200240, China
b
Clean Power Generation Lab, KEPCO Research Institute, Daejeon 34056, Republic of Korea
c
School of Nano & Advanced Materials Engineering, Changwon National University, Changwon 51140, Republic of Korea

ARTICLE INFO ABSTRACT

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Keywords We compare the effects of long-term steam oxidation behavior in two commercial 9% Cr tempered martensite
Heat resistant steel steels with (T92) and without (T91) tungsten at 600–700 °C up to 20,000 h. Microstructural investigations re-
Oxidation veal abnormal grain and oxide scale growth after decomposition of Cr23C6 via oxidation in T91, while the tung-
Oxide scale sten-rich Laves phase in T92 restricts grain growth and assists the formation of a continuous chromite oxide scale.
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Precipitation The findings suggest how formation of Laves phase aids oxidation resistance in heat resistant steels.
Laves phase
Grain growth
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1. Introduction
9–12% Cr tempered martensite ferritic (TMF) steels are widely used
as heat exchanger tubes in thermal power plants [1,2]. Solid solution el-
ements (i.e., Cr, W, Mo, etc.), precipitates, and fine tempered martensite
grains facilitate durability despite creep and oxidation under high-tem-
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over long periods (~40,000 h). However, the underlying details are not
yet known. Since tungsten favored the precipitation of W-Laves in the
TMF structure rather than the formation of a protective surface layer
[11,23,24], it seems reasonable to assume that W-Laves affect oxide
scale formation. Therefore, the purpose of this study is to clarify the pre-
cipitation effect on oxide scale and grain growth in T91 and T92 HRS

perature/pressure steam [3,4]. Optimizing the alloying elements and
heat treatment conditions to obtain fine and stable precipitates is the
key to improving the creep properties of TMF steels [5–7]. For example,
tungsten (W) alloying can stabilize the coarsening of Cr23C6 by the for-
mation of W-rich Laves phase (W-Laves) during high-temperature expo-
sure [8,9]. Increasing alloy concentration and/or reducing grain size are
alternatives for enhancing oxidation resistance, as they can form a pro-
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upon high-temperature steam exposure.
2. Material and method
Samples of 20 × 20 × 5 mm3 were cut from as-received T91 and
T92 tubes purchased from Nippon Steel & Sumitomo Corporation (com-
position in Table 1). The initial dispersions of Cr23C6 within the tem-

tective chromia/chromite oxide scale that covers the metal surface, pre-
venting further oxidation [10–12]. For example, the high alloy content
of austenitic HRS (TP347H, super304H, and HR3C), and shot-peened
9% Cr TMF provides excellent oxidation resistance [13,14].
In previous investigations, precipitates and scales have been treated
as noninteracting entities even at high temperatures [15–18]. For exam-
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pered martensite structures of T91 and T92 are similar. The oxidation
was carried out in our steam oxidation system [25] with steam tem-
peratures of 600, 650, and 700 °C for durations of 10,000, 15,000, and
20,000 h. After the oxidation, cross-sectional samples were prepared for
microstructural investigations by mechanical polishing with a final pol-
ishing with colloidal silica for 2 h.
The morphology, chemical composition, and the phase distributions

ple, Wang et al. reported that the oxidation of Cr23C6 precipitates in an

Fe Si HRS may induce an inhomogeneous distribution of Si in the ox-
ide after approximately 2000 h of steam exposure [19]. Indeed, reports
on the effects of precipitation on the oxide scale are few.
TMF HRS with (T92) and without (T91) W are two commercial 9%
Cr steels that have been applied in power plants for decades [20–24].
A review [11] shows that T92 steels have superior oxidation resis-
tance compared to T91 steels after steam exposure at 600 °C–700 °C
of the oxide layer and matrix were examined by scanning electron
microscopy (SEM) (JSM-5610, equipped with an AZteclive EDS sys-
tem), and electron backscattered diffraction (EBSD) (TESCAN-MIRA II
LMH equipped with TSL OIM system). Samples for transmission elec-
tron microscopy (TEM) analyses were prepared by face-to-face bond-
ing, dimpling, and ion-milling. TEM observations were carried out on a
CM200FEG and a JEM-2100F at 200 keV. Selected area diffraction pat-
tern (SADP) with energy dispersive spectroscopy (EDS) were used to
identify the precipitates and the oxide phase.

⁎ Corresponding authors.
E-mail addresses: yliu23@sjtu.edu.cn (Y. Liu); keesamgg@gmail.com (K. Shin)
1
These authors contributed equally to this work.

https://doi.org/10.1016/j.matchar.2020.110497
Received 7 January 2020; Received in revised form 9 May 2020; Accepted 7 July 2020
H. Ma et al.
Table 1
Chemical composition of T91 and T92 steel (wt%).
C Si Mn P S
T91 0.12 0.50 0.50 ≤0.02
T92 0.12 0.50 0.50 ≤0.02
3. Results and discussion
Fig. 1 is the EBSD-EDS images showing the phases and element dis-
tributions in the scale formed on the surface of T91 and T92 steel after
steam oxidation at 700 °C for 20,000 h. For the T91 sample, an outer
light, a middle light-dark and an inner discontinuous green layer (Fig.
1a), which show the compositional features of enrichment in Fe O,
containment of Cr O and enrichment in Cr O, respectively, are ob-
served (Fig. 1b). The outer and middle layers are mostly a mixture of
hematite and magnetite (H+M). The inner layer is confirmed to be the
chromite (C) phase [26,27]. For T92 samples, an H+M layer and a con-
tinuous C layer are formed on the surface (Fig. 1c and d). In the ox-
ide-metal (O-M) interface, a coarse grain layer (CGL) can be identified
in the matrix region of T91 steel (marked in Fig. 1a). In addition, the
CGL seems to be cut off when the discontinuous C layer appears on the
exposed fine grain matrix. By contrast, no CGL is observed in the T92
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samples.
The CGL in the matrix region is further confirmed by EBSD with
high magnification mapping (Fig. 2). In the lower part of Fig. 2a–b,
the typical microstructure of tempered martensite [28–31] is appar-
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ent, i.e., prior austenite grains with a substructure of lath, sub-grains
and dislocation cells which are mostly contained by the low angle
grain boundaries (LAGB). In contrast, a CGL (dashed line marked re-
gion in Fig. 2a) without LAGB is observed in the T91 samples, indi-
cating the appearance of a rapid grain growth accompanied by a re-
covery of the substructure during the long-term high-temperature expo-
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sure. In Fig. 2b, the LAGB delineated by the dashed line region is de-
creased compared to the lower part of the tempered martensite region,
indicating that the grain recovery may have occurred without significant
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Fig. 1. Combined EBSD phase map (a, c) with corresponding EDS mapping (b, d) of the oxide scale formed on T91 and T92 after steam exposure at 700 °C for 20,000 h. (a, b) show an
H+M+discontinuous C layers on T91. (c, d) show the H+M+C layers on T92.
Materials Characterization xxx (xxxx) xxx-xxx
Cr Ni V Nb Mo W
≤0.01 9.00 ≤0.40 0.08 0.15 1.00 –
≤0.01 9.00 ≤0.40 0.08 0.15 0.50 1.50
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grain growth, which is designated as the recovered grain layer (RGL)
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hereafter.
The average thickness and grain size of the CGL and RGL are shown
in Fig. 3a and b, respectively. For T91 steel, the CGL has a grain size of
~15 μm and ~60 μm after oxidation at 650 °C and 700 °C, respectively.
The grain size is dependent on the temperature, but not on the exposure
time (Fig. 3a–b). For T92 specimens, the grain size of the RGL is ~5 μm,
also independent on exposure time, but with relatively rapid coarsening
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at 700 °C.
Fig. 4 is the SEM secondary electron (SE) and back-scattered elec-
tron (BSE) images of the T91 and T92 specimens after steam exposure
at 650 °C for 15,000 h. In Fig. 4a, numerous Cr-rich precipitates (con-
firmed to be Cr23C6, see below) are distributed along the GB and in the
grain interior (GI) of the matrix region. These are hardly present in the
CGL, indicating the decomposition of Cr23C6 during high-temperature
steam oxidation. Moreover, the observed Cr23C6 precipitates in the CGL
are mostly distributed in the GI and are rare in GB (Fig. 4c). The con-
centration of Cr in GB Cr23C6 is much lower than that of the GI one (1#
and 2# in the inset of Fig. 4c), suggesting a high decomposition rate
of Cr23C6 in GB, which will be discussed later. The corresponding BSE
image shows a similar contrast between the precipitates and the ma-
trix (Fig. 4b), indicating the absence of Mo-rich Laves phase [28,30] in
these T91 samples.
In T92 samples (Fig. 4c–d), two kinds of precipitates, with different
contrasts of light and dark (i.e., red and green shading, respectively),
are observed throughout the microstructure in the deep matrix. These
are interpreted to be the W-rich Laves and Cr-rich Cr23C6 [29,31], re-
spectively (1# and 2# in the inset of Fig. 4f). However, it is difficult to
find Cr23C6 precipitates in the RGL, indicating its decomposition during
high-temperature exposure. In addition, it is easy to find the W-Laves in
the C layer as shown in Fig. 4e.
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Fig. 2. EBSD pole figure with the highlighted LAGB images showing the grain features at the oxide-metal interface region of T91 and T92 after steam exposure at 650 °C for 15,000 h:
(a) a coarse-grained layer (CGL) on T91 and (b) a recovered grain layer (RGL) in T92. Black line: high angle grain boundary (HAGB), Red line: low angle grain boundary (LAGB). (For
interpretation of the references to color in this figure legend, the reader is referred to the web version of this article.)
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Fig. 3. Thickness evolution of CGL on T91 (a), and average grain size in CGL and RGL of T91 and T92 (b).

Fig. 5a–d are the TEM images recorded at representative regions of to the matrix, the Cr-rich Cr23C6 and W-Laves are the dominant precip-
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the O-M interface. Precipitates in T91 samples (Fig. 5a) are confirmed
to be the Cr23C6 (Fig. 5e), which mostly appear within the grain in
the CGL and throughout the microstructure in the tempered martensite
(TM) matrix. In addition, none of the substructures of dislocations and
LAGB is observed in the CGL, which further confirms the grain recovery
and growth.
The high contrast precipitates in the C layer and RGL of the T92
samples (Fig. 5b–c) are confirmed to be the W-Laves (Fig. 5f). The
W-Laves is observed to be surrounded by fine FeCr2O4 (Fig. 5g) inside
the C layer (Fig. 5b). It is difficult to find the original Cr23C6 in the RGL
of the T92 specimens, which is consistent with the SEM results. Down
itates (Fig. 5d). These findings further confirm the decomposition of
Cr23C6 and the stabilization of the W-Laves in the RGL of the T92 steel
during high-temperature steam exposure. One remarkable thing is that
no evidence of Cr23C6 decomposition is observed in the deep matrix.
Therefore, the decomposition of the Cr23C6 in CGL and RGL may be re-
lated to the formation of the C layer.
The Cr23C6 was formed during the tempering of 9% Cr TMF HRS,
which showed a low coarsening rate during long-term exposure at high
temperature. Nucleation and fast growth of Mo-rich Laves are gener-
ally observed under exposure conditions similar to those tested here. Re-
placing the Mo with W in HRS steels may promote nucleation and re

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H. Ma et al. Materials Characterization xxx (xxxx) xxx-xxx

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Fig. 4. SEM images of the O-M interface regions in the T91 (a–c) and T92 (d–f) after steam exposure at 650 °C for 15,000 h. (a, d) and (b, e) are SE and BSE images of the same region,
respectively. (c) and (f) are magnified SE images of the marked regions in (a) and (d), respectively. Insets in (c) and (f) are the averaged EDS results.

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Fig. 5. TEM images (a–d) with corresponding SADP and EDS (e–g) showing the precipitates' features in T91 and T92 after steam exposure at 650 °C for 15,000 h: (a) Distribution of
un-decomposed Cr23C6 in the CGL and matrix in the T91 sample. Precipitation of W-Laves at (b) chromite layer and (c) recovered grain layer (RGL) in T92. (d) Co-existence of Cr23C6 and
W-Laves in the matrix close to the RGL region of T92 after exposure. (e–f) SADP of Cr23C6, W-Laves, and FeCr2O4 with corresponding EDS results, respectively.

tard the coarsening of W-rich Laves during exposure to temperatures face area involved in GB is a widely accepted method of enhancing the
over 600 °C [4,8]. In addition, the precipitates' pinning of dislocations, steam oxidation resistance of HRS [13,14,25,38].
substructures, and GBs to delay recovery and annihilation of dislocation Accordingly, we believe that the formation of the H+M layers is
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during high-temperature exposure is considered to be the main strength-
ening mechanism of HRS [32–34].
It is known that oxidation is a diffusion-controlled process that in-
volves the inward diffusion of O with the outward diffusion of Cr, Fe, Ni,
and Si in the metal surface layer when steel is exposed to a high-temper-
ature oxidizing environment (Fig. 6a) [35]. Formation of defects and
GBs in the bulk metal are considered to be an efficient path [36,37]
for the outward diffusion of Cr to form the fine, dense FeCr2O4 and/
or Cr2O3 that protects the metal from rapid oxidation [10,11]. In ad-
dition, refinement of the grain size to increase the fraction of the sur
the result of the outward diffusion of Fe that was oxidized by the O
ions in both T91 and T92 samples. As shown in Fig. 6b, when the T91
samples were exposed to high-temperature steam (>600 °C), the oxida-
tion kinetics drive the outward diffusion (like “pumping”) of Cr from
the metal through the GBs of the TM structure. This requires that the
Cr23C6 decompose to release Cr, which is verified by the SEM-EDS-EBSD
results that the concentration of Cr in GB is lower than in the GI (in-
set in Fig. 4c), and that the Cr concentration decreases in the order
(H+M)+C > matrix > CG layer (Fig. 1b–d, and the inset of Figs.
4c and 3f). We also see that the pinning effect of the precipitates is
reduced, which finally results in the easy recovery and growth of the

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H. Ma et al.
Fig. 6. Schematic illustration of the oxide scale and microstructure of 9% Cr TMF HRS upon steam oxidation. Inward diffusion of O and outward diffusion of Fe, Cr created the H+M+C
layers (a). Formation of the abnormal oxide layer (H+M+ discontinuous C) and the coarse grains layer due to the decomposition of Cr23C6 in T91 steel (b). Formation of H+M+C layers
shows the stabilization effect of W-Laves in T92 steel (c).
fine TM structure to form the CGL [39,40]. The grain growth decreases
the GB fraction that narrows the efficient diffusion path for Cr to form a
continuous C layer. This may explain the detection of Cr in the M layer,
and the observation of a discontinuous C layer in a relatively fine and
“short” CG region of the O-M interface in the T91 specimens (Fig. 1a).
A similar process may have occurred in the T92 specimens, how-
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ever, since the W-Laves is observed to be fine and stable after steam ex-
posure at 600–700 °C up to 20,000 h. Thus, the W-Laves acts similarly
to Cr23C6 to retard grain recovery and growth, consequently keeping a
large enough fraction of GB to enable the outward diffusion of Cr to
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form a continuous C layer in the scale (Fig. 6c).
4. Conclusions
In summary, two 9% Cr TMF HRS with (T92) and without (T91) W
addition were investigated to determine the effect of precipitation on the
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grain and scale growth after long-term steam oxidation at high-temper-
atures. We found the abnormal formation of a discontinuous chromite
layer on the grown coarse grains layer after decomposition of the Cr23C6
in the surface of T91 samples, whereas there was a growth of a contin-
uous chromite layer on the recovered grain layer with the formation of
W-Laves phases. We found that the precipitation of the stable W-Laves
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phase restricted the grain growth during steam oxidation, which favored
the formation of a chromite layer. This finding is important for the im-
provement of oxidation properties to prevent corrosion and creep by
precipitation control of HRS.
Declaration of competing interest
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All the authors have no interest conflicts.
Acknowledgment
This research was supported by Changwon National University in
2019–2020.
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Data availability
The raw/processed data required to reproduce these findings cannot
be shared at this time as the data are part of an ongoing study.
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