Materials Characterization 101 (2015) 106–113

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Materials Characterization
journal homepage: www.elsevier.com/locate/matchar

Microstructure characterization of heat affected zone after welding in

Mod.9Cr–1Mo steel
K. Sawada a,⁎, T. Hara b, M. Tabuchi a, K. Kimura a, K. Kubushiro c
a
Materials Reliability Unit, National Institute for Materials Science, 1-2-1 Sengen, Tsukuba 305-0047, Japan
b
Surface Physics and Structure Unit, National Institute for Materials Science, 1-2-1 Sengen, Tsukuba 305-0047, Japan
c
IHI Corporation, 1, Shin-nakahara-cho, Isogo-ku, Yokohama 235-8501, Japan

a r t i c l e i n f o a b s t r a c t

Article history: The microstructure of the heat affected zone after welding was investigated in Mod.9Cr–1Mo steel, using TEM
Received 26 September 2014 and STEM-EDX. The microstructure of thin foil was observed at the fusion line, and at the positions of 0.5 mm,
Received in revised form 26 December 2014 1.0 mm, 1.5 mm, 2.0 mm, 2.5 mm, 3.0 mm and 3.5 mm to the base metal side of the fusion line. Martensite struc-
Accepted 18 January 2015
ture with very fine lath and high dislocation density was confirmed at all positions. Twins with a twin plane of
Available online 20 January 2015
(112) were locally observed at all positions. Elemental mapping was obtained for all positions by means of
Keywords:
STEM-EDX. Inclusions of mainly Si were formed at the fusion line but not at the other positions. No precipitates
Mod.9Cr–1Mo steel could be detected at the fusion line or at the position of 0.5 mm. On the other hand, MX particles were observed at
Welding the positions of 1.0 mm, 1.5 mm, 2.0 mm, 2.5 mm, 3.0 mm and 3.5 mm even after welding. M23C6 particles were
FGHAZ also confirmed at the positions of 2.0 mm, 2.5 mm, 3.0 mm and 3.5 mm. Very fine equiaxed grains were locally
Nonequilibrium microstructure observed at the positions of 2.0 mm and 2.5 mm. The Cr content of the equiaxed grains was about 12 mass%,
although the martensite area included about 8 mass% Cr.
© 2015 Elsevier Inc. All rights reserved.

1. Introduction region. However, this may be not nature of creep strength of

Mod.9Cr–1Mo steels (9Cr–1Mo–V–Nb–N) are widely used for com-
ponents of thermal power plants worldwide. Recently, allowable stress-
es of Mod.9Cr–1Mo steels were reviewed in Japan because the creep
strength of Mod.9Cr–1Mo steel decreases in the long term [1,2]. The
creep strength of Mod.9Cr–1Mo steel welds was lower than that of
the base metal in the long term since the drop in creep strength was
larger in the welds than in the base metal in the long term. The long-
term creep data of Mod.9Cr–1Mo steel welds is not enough for the
safe design of components. Yaguchi et al. reported [3] the evaluation
of long-term creep strength of Mod.9Cr–1Mo steel welds, collecting
creep data from eight organizations in Japan. They proposed master
curve for creep rupture data of welds by using region splitting analysis
method. In the method, creep rupture data are split into high stress
and low stress regions using a boundary stress. The creep data for low
stress regions are not enough because the longest creep data of
Mod.9Cr–1Mo steel welds is about 30,000 h at 600 °C which is steam
temperature of ultra-supercritical power plants. Yaguchi et al. com-
pared the creep strength of base metal and that of welds. It can be ex-
pected from the comparison that the creep strength of welds will be
larger than that of base metal after 100,000 h at 650 °C although the
creep strength of welds is lower than that of base metal in short term
⁎ Corresponding author.
E-mail address: sawada.kota@nims.go.jp (K. Sawada).
Mod.9Cr–1Mo steel welds because the creep strength of welds basically
low due to type IV cracking in heat affected zone. The contradictory pre-
diction of long-term creep strength may be due to lack of long-term
creep data of welds.
In order to clarify the reason for the large drop in creep strength of
welds, it is very important to understand the microstructure of the
heat affected zone (HAZ) because creep fracture occurs in the HAZ in
the long term [4]. Mod.9Cr–1Mo steels are usually used after post
weld heat treatment (PWHT) after welding. Many works have focused
on the microstructure of the HAZ after PWHT [5–7]. However, the
heating and cooling rates are very high in the case of welding [8,9],
and so a nonequilibrium microstructure tends to be formed after
welding. It is difficult to identify the nonequilibrium microstructure in
the HAZ after PWHT because it can change during PWHT. Therefore, it
is necessary to investigate the microstructure just after welding (with-
out PWHT) in order to understand the nonequilibrium microstructure.
It has been reported [10] that some M23C6 carbides did not dissolve
and remaining M23C6 carbides coarsened at fine-grained HAZ (FGHAZ)
after thermal cycling corresponding to welding in ASME Gr.92 steel. It
has also been reported for Mod.9Cr–1Mo steel [11] that fresh nucleation
of M23C6 carbides with a low Cr/Fe ratio occurred in the HAZ during
cooling after welding. Delta ferrite was observed at the fusion line
after welding in Mod.9Cr–1Mo steel [11].
The Mod.9Cr–1Mo steels have a tempered martensite structure with
high dislocation density after normalizing and tempering. M23C6

http://dx.doi.org/10.1016/j.matchar.2015.01.013
1044-5803/© 2015 Elsevier Inc. All rights reserved.
 K. Sawada et al. / Materials Characterization 101 (2015) 106–113
Table 1
Chemical composition (mass%) of the steel examined.
C Si Mn P S Ni
0.099 0.38 0.44 0.019 b0.001 0.078
Table 2
Chemical composition (mass%) of the weld metal after welding.
C Si Mn P S Ni
0.074 0.16 1.29 0.018 0.001 0.47
carbides and MX carbonitrides are distributed along lath, block, packet
and prior austenite grain boundaries, which means that elements such
as Cr, V, Nb, C and N forming M23C6 carbides and MX carbonitrides are
concentrated along these grain boundaries. These elements can move
short distances during welding because the holding time after heating
is very short in the case of welding. Therefore, it is necessary to focus
on the local area of the microstructure of the HAZ to clarify the nonequi-
librium microstructure after welding.
The purpose of this study was to clarify the nonequilibrium micro-
structure formed in the HAZ after welding (without PWHT), by examin-
ing the local area by TEM and STEM-EDX.
2. Experimental procedures
The material studied was Mod.9Cr–1Mo steel (KA-SCMV28 [12])
plate of 25 mm thickness. The chemical composition of the steel and
weld metal is listed in Tables 1 and 2, respectively. The chemical compo-
sition of the weld metal was measured after welding. The welding was
performed by submerged arc welding (380A, 30 V, travel speed: 28–40
cm/min), using matching filler metal for Mod.9Cr–1Mo steel. The macro-
structure of the welded plate is shown in Fig. 1. The width of the HAZ was
about 2.5 mm at the central part of thickness. A cylindrical specimen was
cut from the central part of thickness to make thin foils for microstructur-
al observations as shown in Fig. 1. Disks were cut from the cylindrical
specimen at positions corresponding to the fusion line and at 0.5 mm in-
tervals to the base metal side of the fusion line. The disks were mechan-
ically and electrochemically polished to make thin foils. The electrolytic
solution was a solution of 3 ml hydrochloric acid and 1 g picric acid in
100 ml of ethanol. The microstructure was observed by TEM (Hitachi
HF2000) operating at an accelerating voltage of 200 kV. Elemental map-
ping was obtained using JEOL JEM-2010F with STEM BF/ADF detectors,
Schottky thermal type emitter and EDS (Bruker XFlash, Silicon drift de-
tector, detector area: 30 mm2, detecting solid angle: 0.13 str., energy
resolution: 127 eV) operating at an accelerating voltage of 200 kV.
3. Results and discussion
3.1. TEM microstructures
Fig. 2 shows TEM microstructures at the fusion line (0 mm) and at
the positions of 0.5 mm, 1.0 mm, 1.5 mm, 2.0 mm and 2.5 mm.
Fig. 1. Macrostructure of welded plate.
107
Cr Mo Cu V Nb Al N
8.42 0.99 0.026 0.19 0.08 0.009 0.059
Cr Mo Cu V Nb Al N
8.53 0.94 0.020 0.22 0.04 0.003 0.039
Martensite structure with high dislocation density was observed at all
positions. Very fine martensite laths were locally observed. Large parti-
cles were also confirmed at the fusion line, which may have been inclu-
sions which were introduced by the welding process because no large
particles were observed at other positions. Dislocation structures inside
subgrains are shown in Fig. 3. A large number of dislocations were ob-
served at all the positions. A very fine lamellar structure like twins
was locally confirmed at the fusion line and at the positions of
0.5 mm, 1.0 mm, 1.5 mm, 2.0 mm and 2.5 mm as shown in Fig. 4. The
lamellar spacing was about several tens of nanometers which is much
smaller than the width of martensite lath (several hundreds of nanome-
ters). Fig. 5 shows the lamellar structure and its electron diffraction pat-
tern at the position of 2.0 mm. The lamellar structure was clearly twin,
with a twin plane of (112). It is well-known that twins are formed in
steels after martensitic transformation if the carbon concentration is
very high [13]. However, the carbon content of the steel in this study
was low, as listed in Table 1. M23C6 carbides are distributed in this
steel after heat treatment. In the case of welding, the M23C6 carbides
will be locally dissolved in the matrix by heating [10], and so the carbon
content is locally high immediately after the M23C6 has dissolved. How-
ever, most of the carbon from the M23C6 moves long distances because
carbon diffuses very quickly during welding. The twins can be formed
due to lower Ms temperature around the local area. If the Cr content is
high, the Ms temperature is decreased. The Ms temperature is locally
low due to the local dissolution of M23C6 because the Cr is included in
the M23C6. Therefore, the high Cr content in the local area caused the
formation of twin.
3.2. Elemental mapping
Elemental maps were obtained from STEM-EDX at the positions
of 0 mm, 0.5 mm, 1.0 mm, 1.5 mm, 2.0 mm, 2.5 mm, 3.0 mm and
3.5 mm as shown in Fig. 6. Red, green, blue, pink and yellow colors de-
note the elemental maps of Cr, Nb, V, Si and Mo, respectively. The ele-
mental maps were superimposed on bright field images at all
positions. The steel studied included M23C6 and MX carbonitrides after
normalizing and tempering [14]. The particles with red color indicate
M23C6 carbides because M23C6 carbides mainly include Cr and C. The
mean main metallic compositions of the particles with red color at the
position of 2.5 mm were Cr: 54.15, Fe: 37.44, V: 0.62 and Mo: 7.79 in
mass percent. These values are very similar to the chemical composi-
tions of M23C6 particles in base metal of ASME T91 steel [14]. The parti-
cles with blue and/or green colors are MX carbonitrides because MX
carbonitrides mainly consist of V, Nb and N. At the fusion line (0 mm),
large particles with pink color were observed as shown in Fig. 6; these
particles were already seen in Fig. 2. However, no particles except for
the large particles were confirmed at the fusion line, indicating that
most of the M23C6 carbides and MX carbonitrides were dissolved by
welding. In the case of welding, the filler metal includes Si as a deoxidiz-
er. Therefore, it is assumed that the large particles with pink color indi-
cate Si oxide. No particles that included Si were observed at other
positions. No particles were detected at the position of 0.5 mm as
shown in Fig. 6, indicating that most of the M23C6 carbides and MX
108 K. Sawada et al. / Materials Characterization 101 (2015) 106–113

Fig. 2. TEM microstructures at fusion line, HAZ and base metal. (a) Fusion line, (b) position of 0.5 mm, (c) position of 1.0 mm, (d) position of 1.5 mm, (e) position of 2.0 mm, (f) position of
2.5 mm.

Fig. 3. Dislocation structure inside subgrain at fusion line, HAZ and base metal. (a) Fusion line, (b) position of 0.5 mm, (c) position of 1.0 mm, (d) position of 1.5 mm, (e) position of 2.0 mm,
(f) position of 2.5 mm.
 K. Sawada et al. / Materials Characterization 101 (2015) 106–113 109

Fig. 4. Lamellar structures at fusion line, HAZ and base metal. (a) Fusion line, (b) position of 0.5 mm, (c) position of 1.0 mm, (d) position of 1.5 mm, (e) position of 2.0 mm, (f) position of
2.5 mm.

carbonitrides were dissolved. It is assumed that the temperature at the
position of 0.5 mm during welding was high enough to dissolve parti-
cles. Large particles with green color were observed at the position of
1.0 mm; these mainly consisted of Nb, indicating that the particles
were Nb-rich MX carbonitrides. Yoshino et al. reported that Nb-rich
MX particles remained after normalizing even when the normalizing
temperature was high enough (e.g., 1150 °C and 1200 °C) in Mod.9Cr–
1Mo steel [15]. In the case of welding, the holding time at high temper-
ature after heating is quite short, so it is difficult for Nb-rich MX particles
to dissolve in the matrix during welding. In addition to large Nb-rich MX
particles, small particles with blue color were also detected at the posi-
tion of 1.5 mm; these mainly included V, indicating that the particles
were V-rich MX. The V-rich MX can be detected after normalizing if
the normalizing temperature is less than 1100 °C [15]. In addition to
the existence of a small amount of V-rich MX, a small amount of Cr-
rich particles (red color) was also observed at the positions of 2.0 mm
and 2.5 mm. The Cr-rich particles were M23C6 because M23C6 particles
mainly include Cr and C. According to phase diagram by Thermo-calc.,
the dissolution temperature of precipitate was estimated to be about
880 °C and 1310 °C for M23C6 and MX, respectively. However, in the
case of welding, heating time is very fast in addition to short holding
time, indicating that it is difficult for precipitates to dissolve. It means
that dissolution temperature will be increased in the case of welding.
Therefore, it is difficult to predict temperature during welding in
terms of dissolution of precipitates. Very fine grains with red color
were observed at the positions of 2.0 mm and 2.5 mm as indicated by
the arrows in Fig. 6. The crystal structure of the fine grains was bcc,
meaning ferrite grains. A large number of M23C6 (red color) and MX

Fig. 5. Twin observed at position of 2.0 mm.

110 K. Sawada et al. / Materials Characterization 101 (2015) 106–113

Fig. 6. Elemental maps at fusion line, HAZ and base metal. (a) Fusion line, (b) position of 0.5 mm, (c) position of 1.0 mm, (d) position of 1.5 mm, (e) position of 2.0 mm, (f) position of
2.5 mm, (g) position of 3.0 mm, (h) position of 3.5 mm.

(blue color) particles were observed at the positions of 3.0 mm and
3.5 mm as shown in Fig. 6. It was reported that M23C6 and MX particles
were distributed along lath, block and packet boundaries in as-received
specimens of Mod.9Cr–1Mo steel [14]. Therefore, many of the M23C6
and MX particles will not dissolve during welding at the positions of
3.0 mm and 3.5 mm. Recovery of lath structure was locally observed
at the position of 3.0 mm as indicated by the arrow. The recovered
lath was different from the fine ferrite grains that included high Cr con-
tent at the positions of 2.0 mm and 2.5 mm because the Cr content of the
recovered lath was the same as that of the matrix.
Fig. 7 shows the main chemical composition of the matrix at each
position by point analysis of EDX. Fifteen points were measured for
each position, and the mean values were used as the data. The Mo and
Si contents do not depend on the position. However, the Cr and V con-
tents of the matrix decrease when the position separates from the fu-
sion line. Number density of particles is shown in Fig. 8. The number
densities of particles were measured in area of 70 to 95 μm2 for each po-
sition using elemental maps. The number of M23C6 and MX particles in-
creases with increasing distance from the fusion line. This increase in
the number of M23C6 and MX particles can cause a decrease in the Cr
and V contents of the matrix because M23C6 and MX mainly include Cr
and V, respectively.
Creep fracture occurs at the FGHAZ of welded joints for high Cr fer-
ritic steels in the long term [16]. The creep strength of the FGHAZ is
 K. Sawada et al. / Materials Characterization 101 (2015) 106–113 111

lower than that of the base metal [17]. According to optical micrographs
[18], the positions of 2.0 mm and 2.5 mm corresponded to the FGHAZ.
The undissolved M23C6 and MX particles at the positions of 2.0 mm
and 2.5 mm shown in Fig. 6 cannot effectively pin the lath and block
boundaries because the locations of these boundaries before welding
change after welding due to reverse transformation. It is difficult to un-
derstand how the fine ferrite grains with higher Cr content at the posi-
tions of 2.0 mm and 2.5 mm affect creep strength because it is not clear
whether these grains remain after PWHT. In future it is necessary to in-
vestigate how fine ferrite grains change after PWHT.

3.3. Mechanism of formation of fine ferrite grains at the positions of 2.0 mm

and 2.5 mm

The main chemical composition was measured for fine ferrite grains
with red color shown in Fig. 6. The main chemical compositions of each
fine ferrite grain and matrix are summarized in Fig. 9. The Cr content
was higher in the fine ferrite grain than in the matrix at the positions
of 2.0 mm and 2.5 mm. The mean Cr content of the fine ferrite grain
Fig. 7. Main metallic compositions of matrix at fusion line, HAZ and base metal.
was 12.4 mass% and 12.1 mass% at the positions of 2.0 mm and
2.5 mm, respectively, although the mean Cr content of the matrix was
8.1 to 8.3 mass%. Fig. 10 shows the phase diagram of Mod.9Cr–1Mo
steel obtained from Thermo-calc. It was confirmed by optical micro-
graph that the FGHAZ was formed at the positions of 2.0 mm and
2.5 mm, indicating that these positions were heated to the temperature
from Ac1 to Ac3. According to Fig. 10, the Ac3 temperature was around
850 °C for 9 mass% Cr steel. The equilibrium phase is α phase, γ phase,
M23C6 and MX at around 900 °C when the Cr content is about 12
mass%. If the M23C6 particles locally dissolve during welding, the local
area of the matrix includes high Cr content immediately after heating.
The local area contains no carbon because carbon diffuses very quickly
during welding. For example, the diffusion coefficient at 877 °C can be es-
timated to be 1.83 × 10−10 m2/s and 3.31 × 10−15 m2/s for carbon and
chromium in α iron based on literature data [19,20]. In this case, it is pos-
sible that the Cr content of the local area becomes about 12 mass%, indi-
cating that equilibrium α phase is locally formed after heating. The α
phase can remain because the cooling rate is quite high after welding.
The heating rate dependence of transformation temperature was investi-
gated in Mod.9Cr–1Mo steel by measuring thermal expansion (sample
size: φ3 mm, 10 mm length). The Ac1 and Ac3 temperatures were
881 °C and 969 °C, respectively when the heating rate was 50 °C/s,
Fig. 8. Number density of particles at fusion line, HAZ and base metal.
although the Ac1 and Ac3 temperatures were 839 °C and 893 °C,

Fig. 9. Main metallic compositions of matrices and fine ferrite grains at positions of 2.0 mm and 2.5 mm.
112 K. Sawada et al. / Materials Characterization 101 (2015) 106–113
Fig. 10. Phase diagram of the steel studied by Thermo-calc.
respectively for slow heating (1 °C/s). Therefore, in the case of welding, all
of phase boundaries in Fig. 10 will be moved to high temperature region.
However, it may be possible to discuss about the local presence of α
phase depending on the local Cr content as mentioned above.
4. Conclusions
The microstructure of the heat affected zone after welding was inves-
tigated in Mod.9Cr–1Mo steel, focusing on dislocation structure and the
distribution of precipitates. The results are summarized as follows.
1. Martensite structure with very fine lath and high dislocation density
was observed in the heat affected zone after welding.
2. Twins with a twin plane of (112) were locally observed in the heat
affected zone. The presence of twins did not depend on distance
from the fusion line.
3. Si-rich inclusions were observed at the fusion line. MX particles were
confirmed at the positions of 1.0 mm, 1.5 mm, 2.0 mm, 2.5 mm,
3.0 mm and 3.5 mm even after welding. M23C6 particles were ob-
served at the positions of 2.0 mm, 2.5 mm, 3.0 mm and 3.5 mm.
4. Fine ferrite grains with high Cr content were formed after welding at
the positions of 2.0 mm and 2.5 mm. The mean Cr content of the fine
ferrite grains was about 12 mass% although the Cr content of mar-
tensite was about 8 mass%.
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