Materials and Design 190 (2020) 108570

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Materials and Design

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Insight into Type IV cracking in Grade 91 steel weldments

Yiyu Wang ⁎, Rangasayee Kannan, Leijun Li
Department of Chemical and Materials Engineering, University of Alberta, Edmonton, Alberta T6G 2V4, Canada

H I G H L I G H T S G R A P H I C A L A B S T R A C T

• Heterogenous fine-grained strucuture

belonging to the intercritical heat-
affected zone degraded faster than the
other regions.
• Localized C and Cr inhomogeneities in
the matrix weakened intercritical heat-
affected zone.
• Localized high stress triaxiality around
coarsened precipitates induced cavity
nucleation at the triple juctions of grain
boundaries.

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

Article history: In this work, an insight into the premature Type IV cracking was undertaken to clarify its mechanisms in Grade 91
Received 21 November 2019 steel pipe weldments. High-resolution microscopy observations of the as-welded heat-affected zone (HAZ) re-
Received in revised form 15 February 2020 veal that the commonly recognized fine-grained region susceptible of cracking on the edge of HAZ belongs to
Accepted 15 February 2020
the inter-critical HAZ (ICHAZ), rather than the fine-grained HAZ (FGHAZ). Instrumented indentation tests un-
Available online 18 February 2020
cover that the ICHAZ is the weakest region across the weld, exhibiting the largest displacement and the lowest
Keywords:
hardness in three thermal stages. Localized deformation of matrix grains and high stress triaxiality in the
Grade 91 steel weldment ICHAZ promoted nucleation of creep cavities along grain boundaries. This localized deformation was induced
Type IV cracking by the creep strength mismatch of matrix grains with different Cr concentrations. Cavity-free regions exhibit a
Creep rupture mechanism relatively homogenous Cr distribution, whereas, an inhomogeneous Cr distribution is observed in the cavity-
Heat affected zone containing regions. It is believed that this local Cr inhomogeneity in the ICHAZ is caused by the partial dissolution
Characterization of Cr-rich M23C6 carbides and an insufficient homogenization during rapid welding thermal cycles.
© 2020 The Authors. Published by Elsevier Ltd. This is an open access article under the CC BY license (http://
creativecommons.org/licenses/by/4.0/).

1. Introduction
The infamous Type IV cracking has been widely reported as a signif-
icant challenge for applications of 9Cr creep resistant steels in advanced
fossil fuel fired power plants (service temperature above 600 °C) [1–5].
This cracking is commonly observed as a premature failure in the 9Cr
steel weldments. It is reported that Grade 91 steel weldments have
⁎ Corresponding author.
E-mail address: yiyu@ualberta.ca (Y. Wang).
failed below one thousand hours at 650 °C under creep tests [6,7],
which is significantly lower than that of base metal. The Type IV crack-
ing occurred not only in 9Cr steel joints (P91-P92 [8]), but also in other
dissimilar metal welds, for example, 9Cr-Inconel 617 [9]. To improve
creep lifetime of 9Cr steel weldments, creep rupture mechanism of the
Type IV cracking needs to be fully understood. Although many works
have been conducted, there are still some uncertainties, which are be-
lieved to be caused by many factors, including its high structural com-
plexities in heterogenous heat-affected zone (HAZ) with only a few
millimeters thickness, sample preparation, the limited resolution of

https://doi.org/10.1016/j.matdes.2020.108570
0264-1275/© 2020 The Authors. Published by Elsevier Ltd. This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/).
2 Y. Wang et al. / Materials and Design 190 (2020) 108570
optical microscope, and inconsistent hardness measurements. Two
major uncertainties include: (a) Inconsistent reporting the creep rup-
ture location; (b) The critical structure feature responsible for the
Type IV cracking is still under debate.
Fine-grained HAZ (FGHAZ), intercritical HAZ (ICHAZ), and even
over-tempered base metal have been reported as the fracture location
of the Type IV cracking by different researchers [5,10,11]. It is believed
that this location inconsistency is caused by the fact that no physical
boundaries exist between these three regions. The region with the low-
est hardness value is normally considered as the cracking susceptible re-
gion [5,12,13]. However, hardness values of these three regions are
significantly affected not only by the pre-weld heat treatment of base
metal, welding parameters, such as pre-heat and heat input, and the
post-weld heat treatment (PWHT), but also by hardness measurement
procedure itself [14]. It was reported that the Type IV cracking shifted
from the FGHAZ/ICHAZ to over tempered base metal when applying a
PWHT cycle consisting of re-austenitizing followed by tempering in-
stead of the conventional tempering from the as-welded condition
[15]. Physical simulation of heat-affect zone has been conducted to
“magnify” the HAZ microstructure and study creep properties of subre-
gions in the HAZ [16,17]. Microstructure of individual CGHAZ, FGHAZ,
and ICHAZ can be reproduced when the key simulation parameters, in-
cluding heating rate, peak temperature, and dwell time at peak temper-
ature, are carefully controlled. Another challenge for studying the
simulated HAZ is that their creep deformation behavior might be differ-
ent from that of the actual HAZs due to the absence of constraint and
stress triaxiality from the neighboring strong weld metal and base
metal. Therefore, to track the exact location of the Type IV cracking sus-
ceptible region, microstructure evolutions and hardness of sub-regions
in the HAZ of actual welds under three thermal stages, including as-
welded, after post weld heat treatment, and after creep testing, should
be systematically and quantitatively analyzed by using high-resolution
characterization and testing techniques.
Coarsening of precipitates, especially M23C6 carbides and Laves
phase [18], in the FGHAZ and ICHAZ was considered as the main reason
responsible for creep strength degradation in Type IV cracking
[2,3,19,20]. Improving the thermal stability of M23C6 carbides by replac-
ing partial carbon with boron was reported to have improved creep
strength of both the base metal and welds [20–22]. On the other hand,
fine-grained structure was also considered as the key structure feature
Fig. 1. Photographs showing (a) welding setup for the 1-inch thick Grade steel pipe [27] and (b) cross-section of the entire pipe weld [24]. Optical macrographs showing typical examples of
(c) the as-welded HAZ and (d) the HAZ fractured with the Type IV cracking after creep testing (PWHT at 760 °C-8 h) [25]. The analyzed fine-grained region was highlighted by the red star in (c).
reducing the creep resistance. It is reported that fine prior austenite
grain size in the FGHAZ promotes a faster recovery rate of dislocations
and a higher coarsening rate of subgrains [23]. Our recent works
[24,25] found that the intercritical structure of mixed over-tempered
martensite (ferrite) and newly un-tempered martensite, and partially
dissolved precipitates is the key factor responsible for not only the
Type IV cracking in the HAZ, but also Type I cracking in the weld
metal after PWHT at high-temperature above A1.
This work aims to clarify the two uncertainties in the Type IV crack-
ing mechanism by conducting detailed structure analyses on the
welded joints under three thermal stages. High-resolution characteriza-
tion tools, including field emission SEM, instrumented indentation tes-
ter, electron backscatter diffraction, and auger electron spectroscopy,
were used to locate the Type IV cracking susceptible region and to quan-
tify its key structural feature. A finite element analysis with a
microstructure-based model was also conducted to study fracture
mechanism of the observed cracking.
2. Materials and methods
ASTM A387 Grade 91 steel pipe, used as the base metal, had a
219 mm outer diameter (OD) and 29 mm thickness. It had been normal-
ized for 8 min at 1060 °C and tempered for 45 min at 786 °C, in accor-
dance with the ASTM A387 Standard [26]. Flux cored arc welding
(FCAW) and gas tungsten arc welding (GTAW) were used to weld two
124 mm long pipes with a 60° double-V weld groove and 1.5 mm root
face, respectively. The welding setup is shown in Fig. 1a. The FCAW pa-
rameters for the filling passes were 1.0 kJ/mm heat input, 0.292 m/min
linear travel speed, 27 V arc voltage, and 7.62 m/min wire feed speed.
The full welding parameters were described in detail in Ref. [25]. Chem-
ical compositions of the base metal, GTAW filler metal ER90S-B9 and
FCAW filler metal ER91T1-B9 are presented in Table 1. The photograph
in Fig. 1b shows the cross-section of the entire pipe weld. The measured
width of the HAZ is 3 mm. The welds were post-weld heat treated at
760 °C for 2 h. Cross-weld samples extracted from the welds after
PWHT had a cross section of 8.8 × 12.7 mm and an effective gauge
length of 84 mm. They were creep tested at 650 °C with a stress of
70 MPa. The cross-weld specimen failed with the Type IV cracking
after 649 h with a total creep strain of 1.2% over the gauge length.
 Y. Wang et al. / Materials and Design 190 (2020) 108570 3

Table 1
Chemical composition of Grade 91 base metal and filler metals (wt%).

Materials C Cr Mo Mn Si Ni Al V Nb S P N

ER90S-B9 GTAW 0.097 8.830 0.928 0.560 0.250 0.307 0.002 0.197 0.064 0.004 0.006 0.030
E91T1-B9 FCAW 0.100 8.830 0.880 0.790 0.280 0.550 0.001 0.200 0.030 0.008 0.020 0.050
Base metal 0.110 8.470 0.940 0.370 0.370 0.080 0.002 0.190 0.071 0.002 0.016 0.048

Fig. 1 shows examples of the as-welded weldment and the weld with
the Type IV cracking after creep testing.
The HAZ specimens were extracted from weldments in the as-
welded condition, after PWHT, and after creep tests. To locate the crack-
ing susceptible region, instrumented indentation tests were conducted
on specimens for each condition by using a Fischerscope H100C with a
standard diamond pyramid Vicker's indenter at ambient temperature.
The tests were carried out in the load-controlled mode with a peak
load of 500 mN applied over a period of 20 s, then holding at 500 mN
for 10 s, followed by the unloading step. The load-depth curves were an-
alyzed using the Oliver and Pharr analysis for hardness values [28]. For
microstructure analyses, HAZ specimens were prepared by using a con-
ventional mechanical polishing method with a final polishing of
0.02 μm colloidal silica. Microstructure of the base metal and HAZ was
characterized by a Zeiss Sigma field-emission gun SEM (FESEM). The
polished HAZ specimens for FESEM analysis were etched with 10%
Nital for 3 min. Electron backscatter diffraction (EBSD) analysis was con-
ducted on the FESEM equipped with an Oxford AZtec system under 20 kV
accelerate voltage, 60 μm objective aperture, and step size of 0.3 μm for
PWHT-ed samples and 0.15 μm for crept samples. The EBSD data was
post-processed with the Channel 5 software package. Low angle grain
boundaries (LAGBs, misorientation b10°) and high angle grain bound-
aries (HAGBs, misorientation ≥10°) were distinguished by the scalar mis-
orientation between adjacent pixels. This 10° criterion was chosen based
on crystallographic features of low-carbon martensite [29,30]. Matrix
grain size divided by HAGBs was measured with the grain boundary
map by using the line intercept method. Local chemistry analysis was
conducted on the crept HAZ sample by using the Auger electron spec-
troscopy (AED, JEOL-9500F). The accelerating voltage and emission cur-
rent for both the SEM and Auger imaging were 10 kV and 10 nA,
respectively. Ar ion sputtering was applied for 60 s after the secondary
electron imaging and before acquiring the maps to ensure the surface
was free from any contamination. The intensity of each pixel in the
Auger image was calculated by (P-B)/B, where P and B are the peak
and background intensity, respectively. Such intensity definition helps
to reduce the edge effect of island or dot features in the microstructure.
To simulate micro-mechanical response within the ICHAZ under the
creep loading condition (70 MPa) at 650 °C, especially the correlation
between stress distribution and cavity nucleation, a finite element
(FE) analysis was conducted with a microstructure-based model built

Fig. 3. Backscatter electron SEM images showing the structure variations within the as-
Fig. 2. An example of a fine-grained region on the edge of the HAZ under optical welded ICHAZ: (a) the high-temperature end close to FGHAZ; (b) the low-temperature
microscope, which belongs to the ICHAZ under the SEM in the as-welded HAZ: end close to base metal. The large contrast in BSE images shows the Cr/Mo
(a) optical micrograph; (b) SEM BSE micrograph. inhomogeneity which is caused by the partial dissolution of precipitates.
4 Y. Wang et al. / Materials and Design 190 (2020) 108570
from the observed typical ICHAZ microstructure. The model was gener-
ated from a SEM image of the ICHAZ in the crept specimen by the ImageJ
and Matlab software. Three structural components, including soft
grains, hard grains, and precipitates, were considered in the model.
The Young's modulus E (MPa) at 650 °C of the soft grains and hard
grains were 9,491 and 25,394, respectively. The FE analysis was con-
ducted under the plane strain condition with the COMSOL Multiphysics
simulation software. A fixed constraint was applied on the bottom edge.
A pressure force of 70 MPa was applied on the top edge.
3. Results
3.1. Structural variations within the as-welded ICHAZ
Based on the metallurgical definition of heat affected zone, the most
notable structure difference between the FGHAZ and ICHAZ is existence
of the un-transformed over-tempered martensite grains in the ICHAZ,
but not in the FGHAZ. Distinguishing them by conventional optical obser-
vations with a limited resolution may lead to a wrong conclusion. An ex-
ample is shown in Fig. 2. The micrograph in Fig. 2a, taken from the
location marked in Fig. 1c, would be normally considered as the FGHAZ
in terms of the typical fine-grained structure. However, the SEM graph
of a similar area in Fig. 2b indicates that it has structural features of the
ICHAZ. Fig. 3 compares the typical microstructure of the ICHAZ in both
the high-temperature end (close to the FGHAZ) and the low-
temperature end (close to base metal). The SEM micrograph in Fig. 3a
presents a mixed structure of newly-transformed prior austenite grains
(a) Loading-unloading history
(c) After PWHT
Fig. 4. Instrumented indentation tests across the welds under three thermal stages: (a) Loading-unloading curve; Load-displacement curve (b) as-welded condition, (c) after PWHT,
(d) after creep testing.
(PAGs) and un-transformed tempered martensite (TM) grains. Fine dis-
persive TM grains exist in the high-temperature end. It can be seen that
some un-dissolved coarse precipitates distributed inside the matrix.
These precipitates are reported to be Cr-rich M23C6 carbides by many
works [6,31,32]. Contrast of the BSE SEM images in Fig. 3 represents
alloying concentrations, especially Cr. White regions are alloying
element-rich regions. It is clear that these white spots are the previous lo-
cations of Cr-rich M23C6 carbides. Since the diffusion rates of large Cr and
Mo atoms are low in the iron matrix, homogenization of dissolved Cr and
Mo is insufficient after rapid welding heating and cooling, which contrib-
utes to a localized alloying inhomogeneity in the ICHAZ. The EDS mea-
surements show the Cr concentration difference between white region
and dark region can reach to 2–4 wt% [33], which is a non-ignorable dif-
ference in terms of the nominal Cr composition (8.83%). It is believed that
this Cr inhomogeneity can have a negative impact on the ICHAZ's creep
resistance which will be explained in the following sections.
3.2. Instrumented indentation testing
Hardness has been approved as a reliable index of creep strength of
9Cr steels [12,34,35]. The instrumented indentation testing has been re-
ported as an ideal method to investigate mechanical properties in small
scale [28,36]. Fig. 4 shows the load-displacement curves of instrumented
indentation tests. The calculated hardness and creep rate from the load-
displacement curves are plotted in Fig. 5. The creep deformation rate is
evaluated by ΔH/Δt for the creep stage (H is the depth/displacement of
the indenter, t is time). In the as-welded condition (Fig. 4b), the loading
(b) The as-welded condition
(d) After creep testing
 Y. Wang et al. / Materials and Design 190 (2020) 108570
(a) Hardness
Fig. 5. (a) Measured hardness and (b) deformation rate by instrumented indentation tests.
and unloading curves show variations in maximum depth of penetration
in each region, which indicates that large variations of deformation resis-
tance exist in these regions, which is caused by the highly-heterogeneous
structures right after welding thermal cycles studied in a previous work
[33]. The fusion zone (FZ) exhibits the lowest displacement and the
ICHAZ shows the largest displacement in all testing stages. The FZ has
the highest hardness of 5.4 GPa, and the ICHAZ exhibits the lowest hard-
ness of 1.4 GPa. Considering the creep rate shown in Fig. 5b, the ICHAZ
experienced the highest deformation rate of 174.6 μm/h. Low creep
strength of those over-tempered martensite probably leads to this ex-
tremely high deformation rate in the as-welded ICHAZ. The FZ and BM
have the lowest creep rate of about 28 μm/h. In the PWHT condition
(Fig. 4c), no significant difference in the maximum depth of penetration
is observed, which implies that all regions have similar strength levels.
Both the hardness (2.2–2.6 GPa) and creep rate (39–46 μm/h) for each
region are quite close, which indicates that the PWHT tempering effect
is sufficient for hardness homogenization. In the crept condition
(Fig. 4d), the variation in maximum depth of penetration is significant,
which means the creep resistance between these regions varies. The FZ
is still the hardest region and the ICHAZ is the softest region (2.1 GPa).
The higher hardness values after creep test than that in the PWHT condi-
tion is likely caused by the accumulated creep strain in the HAZ regions.
Locally the matrix grains were deformed after creep test and the inden-
tation test is very sensitive to microstructure variations. The hardness
distribution trend across these tested regions is consistent with the
other two conditions. For the deformation rate, the ICHAZ still has the
highest value of 24 μm/h, which implies its lowest strength.
3.3. Microstructural evolutions after PWHT and creep testing
Optical macrographs of the HAZ specimens under three thermal
stages are presented in Fig. 6. Structural variations, especially PAG
Fig. 6. Optical images of the welds under three thermal stages: (a) As-welded condition [31]; (b) After PWHT; (c) after creep testing.
5
(b) Deformation rate
size, in the as-welded HAZ are easily observed. After creep testing,
black dots of creep cavities are observed on the outer edge of the HAZ
in Fig. 6c. It is evident that cavities were present in the FGHAZ, ICHAZ,
and over-tempered base metal, but the ICHAZ has the highest number
density of cavities. To examine structural evolutions across the welds,
EBSD analyses were conducted on the PWHT-ed and crept specimens.
Characterization of the as-welded specimen was reported in a previous
work [33]. The PWHT is normally used to reduce hardness differences
between the FZ, HAZ, and base metal, and improve toughness of
welds by homogenizing large structural variations across the welds
[27,37]. Microstructure evolutions across the weld after PWHT
(760 °C-2 h) were characterized by EBSD, shown in Fig. 7. It is notable
that there are still large structure variations even after PWHT. The FZ
still keeps the as-welded microstructure of large PAGs with wide mar-
tensite laths. Due to substructures of martensite packet and blocks, the
measured crystal grain size of the FZ is only about 1.80 ± 1.71 μm.
The CGHAZ in Fig. 7b also shows a coarse-grained structure (average
size: 2.10 ± 2.56 μm). The fractions of HAGBs in both FZ and CGHAZ
are about 35%. Both FGHAZ and ICHAZ in Fig. 7c and d exhibit fine-
grained structure features. The fine grains (average size: 1.79 ±
1.87 μm) in the FGHAZ is due to insufficient grain growth of austenite
at low peak temperatures. However, the fine grains (average size:
1.95 ± 1.73 μm) in the ICHAZ are over-tempered martensite grains
from the base metal and small transformed PAGs. The finer grain size at-
tributed to the higher fractions of HAGBs in the FGHAZ (40%) and ICHAZ
(37%). Base metal (average size: 2.00 ± 1.53 μm) in Fig. 7e shows a
structure of fine equiaxed grains and tempered martensite, which has
the highest fraction (44%) of HAGBs. The kernel average misorientation
(KAM) calculated from the EBSD data measures local plastic strain of
grains due to local variations in lattice orientation, which is a sensitive
indicator of the internal dislocation density of grains. The high KAM
value indicates a high dislocation density in the structure, for example,
6 Y. Wang et al. / Materials and Design 190 (2020) 108570
Fig. 7. EBSD inverse pole figures of sub-regions across the weld after PWHT: (a) FZ;
(b) CGHAZ; (c) FGHAZ; (d) ICHAZ; (e) BM.
un-tempered martensite. The KAM maps across the FZ to the BM are
shown in Fig. 8. Statistical distribution of the KAM values is plotted in
Fig. 11a. It clearly shows that the FZ and CGHAZ establish higher strain
levels with more green-color regions. The misorientation peaks shift
from 0.65° to 0.45° from the FZ to the BM. The normalized KAM values
Fig. 8. EBSD kernel average misorientation maps of sub-regions across the weld after
PWHT: (a) FZ; (b) CGHAZ; (c) FGHAZ; (d) ICHAZ; (e) BM.
Fig. 9. EBSD inverse pole figures of sub-regions across the weld after creep testing: (a) FZ;
(b) CGHAZ; (c) FGHAZ; (d) ICHAZ; (e) BM.
of the FZ and CGHAZ are 1.06° and 1.10°, respectively. The FGHAZ,
ICHAZ, and BM exhibit comparable distributions with normalized
KAM values of 0.95°, 0.98°, and 0.84°, respectively. These results imply
that the tempering at 760 °C for 2 h has a significant tempering effect
on the weld by eliminating excessive dislocations from martensitic
Fig. 10. EBSD kernel average misorientation maps of sub-regions across the weld after
creep testing: (a) FZ; (b) CGHAZ; (c) FGHAZ; (d) ICHAZ; (e) BM.
 Y. Wang et al. / Materials and Design 190 (2020) 108570 7

(a) After PWHT (b) After creep testing

Fig. 11. EBSD kernel average misorientation distribution of sub-regions across the weld (a) after PWHT and (b) after creep testing.

transformation on-cooling. Since the base metal was initially tempered
at 786 °C, an additional tempering from the PWHT further reduced the
dislocation density of over-tempered base metal. Therefore, the KAM
in the over-tempered BM is expected to be the lowest among the
three FZ, HAZ, and BM.
The weld with a Type IV cracking after creep testing is also analyzed
with EBSD for comparison in Fig. 9. It is noted that the location of the an-
alyzed FGHAZ is in the transition region between the FGHAZ and ICHAZ.
The FZ and CGHAZ still exhibit a structure of martensite laths. Fine
equiaxed grains are also observed in both the FZ and CGHAZ. The FZ
has the finest grain size of 0.92 ± 0.83 μm. Relative coarse grain struc-
tures (about 2 μm) with a HAGB fraction of about 55.5% are observed
in the FGHAZ and ICHAZ. The equiaxed shape of matrix grains indicates
recovery and recrystallization occurred in these regions. The KAM maps
in Fig. 10 and distribution profiles in Fig. 11b clearly show that strain en-
ergies of each region can be ranked as FZ N CGHAZ N FGHAZ N ICHAZ. The

Fig. 12. Fractography of the creep ruptured cross-weld specimens with the Type IV cracking.

Fig. 13. EDS mapping analysis of a dimple on fracture surface of the creep ruptured cross-weld specimens with the Type IV cracking.
8 Y. Wang et al. / Materials and Design 190 (2020) 108570

Fig. 14. SEM micrographs showing creep cavities in the Type IV cracking. (a), (c), and (d) are backscatter electron images; (b) is a secondary electron image.

Fig. 15. Local element distribution in the cavity-free region in the ICHAZ after creep testing: (a) SEM image; (b) C map; (c) Cr map; (d) Fe map.
 Y. Wang et al. / Materials and Design 190 (2020) 108570
FZ and CGHAZ still maintain the highest strain levels with the KAM
peaks around 0.5°. Normalized KAM values in the FZ and CGHAZ are
0.85° and 0.73°, respectively. The KAM peaks of the FGHAZ and ICHAZ
in Fig. 11b shrink into a low value of 0.15°. The normalized KAM values
in the FGHAZ and ICHAZ are 0.29° and 0.30°, respectively. It should be
noted that the high KAM region in the FGHAZ is associated with a
creep cavity, which implies that large local deformation occurred during
cavitation. Based on the low KAM values, the FGHAZ and ICHAZ experi-
enced a significant creep strength degradation during creep testing.
Combined with the indentation results in Fig. 4, the ICHAZ has the larg-
est deformation and the highest strain energy reduction during creep
testing, which is considered to be the most susceptible region for the
Type IV cracking.
3.4. Cavitation in the Type IV cracking
The Type IV cracking was considered as a brittle fracture in terms of
the low total creep strain across the gauge length, however, recent re-
search reported that locally it is a ductile fracture within the HAZ
[38–40]. Fig. 12 shows a typical fracture surface of the specimen with
a Type IV cracking. Shallow dimples in Fig. 12b indicate increased
creep rate (deformation) in the tertiary stage of creep testing. Some
large particles, very likely inclusions, are observed inside dimples. The
EDS maps in Fig. 13 presents distribution of the major alloying elements
around a dimple. A large amount of Cr-Mo-rich spots are observed on
the dimple wall, which are likely the Cr-rich M23C6 carbides. These dim-
ple wall carbides indicate there are large local deformation along grain
boundaries during fracture.
Fig. 16. Local element distribution in the cavity-containing region in the ICHAZ after creep testing: (a) SEM image; (b) C map; (c) Cr map; (d) Fe map.
9
Fig. 14 shows creep cavities of the Type IV cracking in the ICHAZ. It is
clear that cavities nucleated along high-angle grain boundaries, espe-
cially triple junctions (Fig. 14c). Deformation and rotation of matrix
grains in Fig. 14b assisted nucleation of cavities. In Fig. 14d, it is evident
that the cavities are always associated with coarse precipitates along
grain boundaries. The nucleated cavities tend to connect with each
other and isolate the central grain from other neighboring grains.
These coarsened precipitates have been identified as the Cr-rich M23C6
carbides or Laves phases [18]. Besides the feature above, one more inter-
esting observation is that there is always one grain which is surrounded
by cavities, experienced a significant deformation, but the neighboring
grains seems to be stronger and didn't deform much. It is believed
that this deformed grain is weaker during creep testing, and its prefer-
ential deformation favors the nucleation of cavities. The observed
strength mismatch of matrix grains should be highly related with the
dissolved C and Cr concentrations. C and Cr distributions in two regions
in the ICHAZ after creep testing, one cavity-free region and another re-
gion with cavities, were analyzed for comparison with the auger elec-
tron spectroscopy mapping in Fig. 15. It shows that in the cavity-free
region, C-rich spots in Fig. 15b are correlated with the carbides observed
in Fig. 15a. Since the nominal C composition of Grade 91 steel is low and
only 0.11 wt%, precipitation of these coarsened carbides have consumed
most of the C, which is one of the most efficient interstitial strengthen-
ing elements in the matrix. The reduced carbon lowered creep resis-
tance of the matrix grains during creep. High Cr spots are observed in
Fig. 15c, which is likely the Cr-rich M23C6 carbides. The Cr distribution
inside matrix grains is quite homogeneous, which indicates that matrix
grains have a comparable strength and would respond similarly without
preferential deformation of individual grains. However, the situation in
10 Y. Wang et al. / Materials and Design 190 (2020) 108570
Fig. 17. A microstructure-based model built from the observed SEM image (a) in the specimen after creep test, including three structural components, (b) precipitates, (c) hard grains, and
(d) soft grains.
the cavity-containing region is significantly different, especially C and Cr
distribution. After a long-term creep test, the distribution of C is highly
inhomogeneous. Carbon concentrated in certain points which correlate
to those coarsened carbides and microcracks. The C concentration in the
matrix itself is low close to the cavity areas. The Cr distribution in
Fig. 16c is inhomogeneous inside matrix grains. This Cr concentration
difference between grains can be 2%, which causes strength mismatch
between matrix grains. Thus, during creep testing, some weak grains
with low Cr concentrations preferentially deformed first, but those
stronger ones with higher Cr concentrations deformed less. These
creep deformation variations among matrix grains eventually cause
local stress concentrations and enhance nucleation of cavities as
shown in Fig. 16a.
4. Discussion
It is well-known that grain size is one of the most important traces for
identifying the different sub-regions within the HAZ. However, the fine-
grained structure in both the FGHAZ and ICHAZ makes it difficult for op-
tical observations. The high-resolution FESEM images in Fig. 3 success-
fully capture the characteristic structure of fine untransformed over-
tempered martensite in the as-welded ICHAZ. The BSE FESEM images
in Fig. 3 also give chemical composition contrast of the structure, which
is important to distinguish the FGHAZ and ICHAZ as well. For example,
undissolved Cr-rich M23C6 carbide is a signature of the ICHAZ and the
BSE image in Fig. 3 clearly shows this feature, which cannot be resolved
by optical observations. The instrumented indentation test used in this
work overcomes some limitations of the conventional hardness
Fig. 18. Finite element analysis of the built micro-mechanic model with 70 MPa pressure load at 650 °C, (a) boundary conditions and mesh, (b) first principal stress, (c) Von Mises stress,
and (d) Stress triaxiality.
indentation test. For example, a large indentation spacing (N150 μm)
with a high loading force (1 kgf) in regular hardness tests only can
cover only a few measurements across the entire HAZ (2–3 mm thick-
ness). Since the transition region between FGHAZ and ICHAZ is
b100 μm, the large indentation spacing may easily skip this region. The
instrumented indentation test can have a quite small indentation spacing
(b50 μm), which can give more data points within the same region. An-
other advantage of the instrumented indentation is that it can give not
only hardness values, but also deformation data of each point, which
can be used for micro-mechanics calculations, such as deformation rate.
In this work, by using these high-resolution tools, the most Type IV crack-
ing susceptible region has been confidently traced back to the ICHAZ.
The next question to be answered is why cavities preferentially nu-
cleated in the ICHAZ. From the stress constraint perspective, it has been
reported that the ICHAZ experienced the largest stress triaxiality factor
[7,11]. From the microstructure point of view, formation of cracks is a
process of accumulating creep cavities. Growing and inter-connection
of nucleated creep cavities lead to formation of microcracks. Therefore,
the relation between stress triaxiality distribution and nucleation of
creep cavities may be worthy of checking. It has been reported that
the nucleation and growth of creep cavities is the dominating reason
for creep strength degradation [5,6]. To investigate nucleation of cavities
in a micro-scale level, a microstructure-based model was built and
shown in Fig. 17. This simplified model contains three main structural
components, the precipitates (only M23C6) in Fig. 17b, the hard grains
(Fig. 17c) which represent the Cr-rich grains observed in Fig. 15, and
the soft grains (Fig. 17d) which represents the Cr-depleted grains ob-
served in Fig. 15. Finite element analysis was conducted with a pressure
 Y. Wang et al. / Materials and Design 190 (2020) 108570 11

Fig. 19. Observed nucleation sites of creep cavities (a) show a consistence with the locations (b) with high stress triaxiality values. Precipitates are highlighted by the letter “P” in (b).

load of 70 MPa at 650 °C. The distributions of first principal stress, von
Mises stress, and stress triaxiality are presented in Fig. 18. Generally,
similar distributions of von Mises stress and first principal stress are ob-
served in the structure. The first principal stress level is higher than the
von Mises stress. Local stress concentration as high as 200 MPa is ob-
served to be associated with precipitates. A higher stress level
(N70 MPa) exists in some of precipitates and adjacent regions. High
stress levels (N100 MPa) are also observed in some triple points of
grain boundaries which are high-angle grain boundaries. Fig. 18d
shows the stress triaxiality distribution in the structure. Points with a
stress triaxiality as high as 7 are observed. Their locations are different
from the points with high stress levels. Some grain boundary triple
points close to precipitates show high stress triaxiality. Fig. 19 shows
an example of stress triaxiality distribution in the microstructure-
based model and an observed creep cavity in the ICHAZ. It is obvious
that the coarse precipitate near the triple point of high-angle grain
boundaries causes a high stress triaxiality in the triple point. A region
with a high stress triaxiality value is also observed at the interface be-
tween precipitate and matrix grain. A small cavity nucleated at the
end of the rod-like precipitates. Grain boundary folded at triple points
promotes nucleation of creep cavities. Therefore, locations with high
stress triaxiality are likely sites for cavity nucleation.
Fig. 20 schematically summaries structural evolutions in the ICHAZ
from the initial state of base metal towards the ultimate Type IV

Fig. 20. Schematic illustration of structural evolutions in the ICHAZ towards the Type IV cracking. The light yellow and dark yellow inside grains indicate the low and high Cr concentrations,
respectively.
12 Y. Wang et al. / Materials and Design 190 (2020) 108570
cracking after creep test. A previous work [24] shows an inhomoge-
neous Cr distribution in the as-received base metal, which causes non-
uniform chemical potentials of austenization. Under the rapid heating
thermal cycle of arc welding, heterogeneous martensite/ferrite-to-
austenite transformation occurred in the ICHAZ, which leads to the
mixed structure of transformed martensite and untransformed but
over-tempered martensite. The insufficient growth of transformed aus-
tenite due to the relatively low peak temperature in the ICHAZ led to a
fine prior austenite grain size with a large fraction of PAG boundaries.
M23C6 carbides preferentially nucleated and grew on those PAG bound-
aries, which lowers its creep resistance by reducing the pinning effect
[6,10]. The multi-level martensite boundaries (lath/block/packet) in
Grade 91 steel play a significant role in maintaining its high creep
strength. Wherever, the fine PAG size also affects the crystallographic
feature of martensitic transformation during cooling. It is observed
that the number of transformed martensite packets was reduced
when the PAG size is below 10 μm [41]. The micrograph in Fig. 2 clearly
shows that the majority of PAGs is b10 μm. Based on the crystallography
in lath martensite, the decreased packet boundaries results in a lower
number of block boundaries. Due to the limited available packet/block
boundaries, M23C6 carbides had to nucleate and gather along the PAGs
instead of a homogeneous distribution. These decreased boundary
strengthening and precipitation strengthening directly lower the
ICHAZ's creep resistance. Meanwhile, the dissolution of Cr- rich M23C6
carbides enhanced the local Cr inhomogeneity in the ICHAZ, as shown
in Fig. 3. The transformed martensite experienced recovery of excessive
dislocations generated during martensitic transformation. Whereas,
those over-tempered martensite experienced extensive recovery and
grain growth since they already underwent the initial recovery process
as the base metal, which led to an increase of high-angle grain bound-
aries. The grain boundary migration during grain growth also pushed
those undissolved but coarsened carbides to the HAGBs. These two dif-
ferent evolution paths in matrix grains differentiate their strain energies
with a heterogeneous grain growth (Fig. 20c). The EBSD KAM in Fig. 8d
roughly shows two levels of strain energies in the PWHT-ed ICHAZ. In
creep testing, the strength mismatch caused by the inhomogeneous Cr
distribution leads to a preferential deformation of weak grains, which
accelerated nucleation of creep cavities. The increased fraction (55%)
of HAGBs in the ICHAZ due to a faster grain growth during creep assisted
carbides' coarsening. The high stress triaxiality caused by those coars-
ened precipitates along the triple junction of high-angle grain bound-
aries, especially M23C6 carbides, further attributed to cavity nucleation.
Figs. 15 and 16 clearly show the effect of Cr distribution on cavity nucle-
ation in two typical regions. Based on the results above, minimizing the
localized alloying inhomogeneity in the as-welded ICHAZ is a flexible
approach to improve creep lifetime of 9Cr steel welds.
5. Conclusions
An insight has been built to clarify the Type IV cracking mechanism
in Grade 91 steel. A detailed structure analysis was conducted on its
welds under three continuous thermal stages. Based on the observa-
tions, the following conclusions are drawn:
(1) Conventional optical observations can cause inconsistencies in
identifying the Type IV cracking region. A careful examination
with high-resolution tools is necessary to distinguish structural
features of the FGHAZ and ICHAZ. Creep cavities were observed
in both the FGHAZ, ICHAZ, and over-tempered base metal, but
the ICHAZ has the highest number density of cavities.
(2) The PWHT at 760 °C for 2 h did significantly reduce the strain
(hardness) differences across the welds. However, structural
variations, in terms of grain morphology and size, still exist
even after the PWHT. These heterogeneities differentiate their
deformation responses in each region during creep testing.
(3) For the short-term Type IV cracking, extensive grain growth in
the FGHAZ and ICHAZ is the direct cause for the creep strength
degradation. Local deformation of matrix grains promotes nucle-
ation and growth of creep cavities. Cr inhomogeneity leads to a
strength mismatch between those grown matrix grains during
creep, which accelerates local deformation and cavity nucleation.
Partial dissolution of M23C6 carbides with insufficient diffusion in
the ICHAZ during rapid welding thermal cycles is the main cause
for this alloying inhomogeneity.
CRediT authorship contribution statement
Yiyu Wang: Conceptualization, Data curation, Formal analysis, In-
vestigation, Methodology, Writing - original draft, Writing - review &
editing. Rangasayee Kannan: Formal analysis, Investigation, Writing -
review & editing. Leijun Li: Conceptualization, Formal analysis, Writing
- review & editing, Funding acquisition, Supervision.
Declaration of competing interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influ-
ence the work reported in this paper.
Acknowledgment
This research work was sponsored by the Natural Sciences and Engi-
neering Research Council of Canada through a Discovery Grant
(RES0020431). The author would like to thank Dr. Andrew Deceuster,
Dr. Bishal Silwal, and Benjamin Griffiths from the Utah State University
are thanked for their help on welding and creep testing experiments. Dr.
Shihong Xu and Dr. Meisam Nouri from the University of Alberta are
thanked for their help on AES and indentation tests.
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