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Materials and Design 190 (2020) 108570

Contents lists available at ScienceDirect

Materials and Design

journal homepage: www.elsevier.com/locate/matdes

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 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-
The infamous Type IV cracking has been widely reported as a signif- ing occurred not only in 9Cr steel joints (P91-P92 [8]), but also in other
icant challenge for applications of 9Cr creep resistant steels in advanced dissimilar metal welds, for example, 9Cr-Inconel 617 [9]. To improve
fossil fuel fired power plants (service temperature above 600 °C) [1–5]. creep lifetime of 9Cr steel weldments, creep rupture mechanism of the
This cracking is commonly observed as a premature failure in the 9Cr Type IV cracking needs to be fully understood. Although many works
steel weldments. It is reported that Grade 91 steel weldments have have been conducted, there are still some uncertainties, which are be-
lieved to be caused by many factors, including its high structural com-
⁎ Corresponding author. plexities in heterogenous heat-affected zone (HAZ) with only a few
E-mail address: yiyu@ualberta.ca (Y. Wang). 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 reducing the creep resistance. It is reported that fine prior austenite
major uncertainties include: (a) Inconsistent reporting the creep rup- grain size in the FGHAZ promotes a faster recovery rate of dislocations
ture location; (b) The critical structure feature responsible for the and a higher coarsening rate of subgrains [23]. Our recent works
Type IV cracking is still under debate. [24,25] found that the intercritical structure of mixed over-tempered
Fine-grained HAZ (FGHAZ), intercritical HAZ (ICHAZ), and even martensite (ferrite) and newly un-tempered martensite, and partially
over-tempered base metal have been reported as the fracture location dissolved precipitates is the key factor responsible for not only the
of the Type IV cracking by different researchers [5,10,11]. It is believed Type IV cracking in the HAZ, but also Type I cracking in the weld
that this location inconsistency is caused by the fact that no physical metal after PWHT at high-temperature above A1.
boundaries exist between these three regions. The region with the low- This work aims to clarify the two uncertainties in the Type IV crack-
est hardness value is normally considered as the cracking susceptible re- ing mechanism by conducting detailed structure analyses on the
gion [5,12,13]. However, hardness values of these three regions are welded joints under three thermal stages. High-resolution characteriza-
significantly affected not only by the pre-weld heat treatment of base tion tools, including field emission SEM, instrumented indentation tes-
metal, welding parameters, such as pre-heat and heat input, and the ter, electron backscatter diffraction, and auger electron spectroscopy,
post-weld heat treatment (PWHT), but also by hardness measurement were used to locate the Type IV cracking susceptible region and to quan-
procedure itself [14]. It was reported that the Type IV cracking shifted tify its key structural feature. A finite element analysis with a
from the FGHAZ/ICHAZ to over tempered base metal when applying a microstructure-based model was also conducted to study fracture
PWHT cycle consisting of re-austenitizing followed by tempering in- mechanism of the observed cracking.
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- 2. Materials and methods
gions in the HAZ [16,17]. Microstructure of individual CGHAZ, FGHAZ,
and ICHAZ can be reproduced when the key simulation parameters, in- ASTM A387 Grade 91 steel pipe, used as the base metal, had a
cluding heating rate, peak temperature, and dwell time at peak temper- 219 mm outer diameter (OD) and 29 mm thickness. It had been normal-
ature, are carefully controlled. Another challenge for studying the ized for 8 min at 1060 °C and tempered for 45 min at 786 °C, in accor-
simulated HAZ is that their creep deformation behavior might be differ- dance with the ASTM A387 Standard [26]. Flux cored arc welding
ent from that of the actual HAZs due to the absence of constraint and (FCAW) and gas tungsten arc welding (GTAW) were used to weld two
stress triaxiality from the neighboring strong weld metal and base 124 mm long pipes with a 60° double-V weld groove and 1.5 mm root
metal. Therefore, to track the exact location of the Type IV cracking sus- face, respectively. The welding setup is shown in Fig. 1a. The FCAW pa-
ceptible region, microstructure evolutions and hardness of sub-regions rameters for the filling passes were 1.0 kJ/mm heat input, 0.292 m/min
in the HAZ of actual welds under three thermal stages, including as- linear travel speed, 27 V arc voltage, and 7.62 m/min wire feed speed.
welded, after post weld heat treatment, and after creep testing, should The full welding parameters were described in detail in Ref. [25]. Chem-
be systematically and quantitatively analyzed by using high-resolution ical compositions of the base metal, GTAW filler metal ER90S-B9 and
characterization and testing techniques. FCAW filler metal ER91T1-B9 are presented in Table 1. The photograph
Coarsening of precipitates, especially M23C6 carbides and Laves in Fig. 1b shows the cross-section of the entire pipe weld. The measured
phase [18], in the FGHAZ and ICHAZ was considered as the main reason width of the HAZ is 3 mm. The welds were post-weld heat treated at
responsible for creep strength degradation in Type IV cracking 760 °C for 2 h. Cross-weld samples extracted from the welds after
[2,3,19,20]. Improving the thermal stability of M23C6 carbides by replac- PWHT had a cross section of 8.8 × 12.7 mm and an effective gauge
ing partial carbon with boron was reported to have improved creep length of 84 mm. They were creep tested at 650 °C with a stress of
strength of both the base metal and welds [20–22]. On the other hand, 70 MPa. The cross-weld specimen failed with the Type IV cracking
fine-grained structure was also considered as the key structure feature after 649 h with a total creep strain of 1.2% over the gauge length.

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).
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 post-processed with the Channel 5 software package. Low angle grain
the Type IV cracking after creep testing. boundaries (LAGBs, misorientation b10°) and high angle grain bound-
The HAZ specimens were extracted from weldments in the as- aries (HAGBs, misorientation ≥10°) were distinguished by the scalar mis-
welded condition, after PWHT, and after creep tests. To locate the crack- orientation between adjacent pixels. This 10° criterion was chosen based
ing susceptible region, instrumented indentation tests were conducted on crystallographic features of low-carbon martensite [29,30]. Matrix
on specimens for each condition by using a Fischerscope H100C with a grain size divided by HAGBs was measured with the grain boundary
standard diamond pyramid Vicker's indenter at ambient temperature. map by using the line intercept method. Local chemistry analysis was
The tests were carried out in the load-controlled mode with a peak conducted on the crept HAZ sample by using the Auger electron spec-
load of 500 mN applied over a period of 20 s, then holding at 500 mN troscopy (AED, JEOL-9500F). The accelerating voltage and emission cur-
for 10 s, followed by the unloading step. The load-depth curves were an- rent for both the SEM and Auger imaging were 10 kV and 10 nA,
alyzed using the Oliver and Pharr analysis for hardness values [28]. For respectively. Ar ion sputtering was applied for 60 s after the secondary
microstructure analyses, HAZ specimens were prepared by using a con- electron imaging and before acquiring the maps to ensure the surface
ventional mechanical polishing method with a final polishing of was free from any contamination. The intensity of each pixel in the
0.02 μm colloidal silica. Microstructure of the base metal and HAZ was Auger image was calculated by (P-B)/B, where P and B are the peak
characterized by a Zeiss Sigma field-emission gun SEM (FESEM). The and background intensity, respectively. Such intensity definition helps
polished HAZ specimens for FESEM analysis were etched with 10% to reduce the edge effect of island or dot features in the microstructure.
Nital for 3 min. Electron backscatter diffraction (EBSD) analysis was con- To simulate micro-mechanical response within the ICHAZ under the
ducted on the FESEM equipped with an Oxford AZtec system under 20 kV creep loading condition (70 MPa) at 650 °C, especially the correlation
accelerate voltage, 60 μm objective aperture, and step size of 0.3 μm for between stress distribution and cavity nucleation, a finite element
PWHT-ed samples and 0.15 μm for crept samples. The EBSD data was (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- (PAGs) and un-transformed tempered martensite (TM) grains. Fine dis-
ated from a SEM image of the ICHAZ in the crept specimen by the ImageJ persive TM grains exist in the high-temperature end. It can be seen that
and Matlab software. Three structural components, including soft some un-dissolved coarse precipitates distributed inside the matrix.
grains, hard grains, and precipitates, were considered in the model. These precipitates are reported to be Cr-rich M23C6 carbides by many
The Young's modulus E (MPa) at 650 °C of the soft grains and hard works [6,31,32]. Contrast of the BSE SEM images in Fig. 3 represents
grains were 9,491 and 25,394, respectively. The FE analysis was con- alloying concentrations, especially Cr. White regions are alloying
ducted under the plane strain condition with the COMSOL Multiphysics element-rich regions. It is clear that these white spots are the previous lo-
simulation software. A fixed constraint was applied on the bottom edge. cations of Cr-rich M23C6 carbides. Since the diffusion rates of large Cr and
A pressure force of 70 MPa was applied on the top edge. Mo atoms are low in the iron matrix, homogenization of dissolved Cr and
Mo is insufficient after rapid welding heating and cooling, which contrib-
3. Results utes to a localized alloying inhomogeneity in the ICHAZ. The EDS mea-
surements show the Cr concentration difference between white region
3.1. Structural variations within the as-welded ICHAZ 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
Based on the metallurgical definition of heat affected zone, the most this Cr inhomogeneity can have a negative impact on the ICHAZ's creep
notable structure difference between the FGHAZ and ICHAZ is existence resistance which will be explained in the following sections.
of the un-transformed over-tempered martensite grains in the ICHAZ,
but not in the FGHAZ. Distinguishing them by conventional optical obser- 3.2. Instrumented indentation testing
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 Hardness has been approved as a reliable index of creep strength of
location marked in Fig. 1c, would be normally considered as the FGHAZ 9Cr steels [12,34,35]. The instrumented indentation testing has been re-
in terms of the typical fine-grained structure. However, the SEM graph ported as an ideal method to investigate mechanical properties in small
of a similar area in Fig. 2b indicates that it has structural features of the scale [28,36]. Fig. 4 shows the load-displacement curves of instrumented
ICHAZ. Fig. 3 compares the typical microstructure of the ICHAZ in both indentation tests. The calculated hardness and creep rate from the load-
the high-temperature end (close to the FGHAZ) and the low- displacement curves are plotted in Fig. 5. The creep deformation rate is
temperature end (close to base metal). The SEM micrograph in Fig. 3a evaluated by ΔH/Δt for the creep stage (H is the depth/displacement of
presents a mixed structure of newly-transformed prior austenite grains the indenter, t is time). In the as-welded condition (Fig. 4b), the loading

(a) Loading-unloading history (b) The as-welded condition

(c) After PWHT (d) After creep testing


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.
Y. Wang et al. / Materials and Design 190 (2020) 108570 5

(a) Hardness (b) Deformation rate

Fig. 5. (a) Measured hardness and (b) deformation rate by instrumented indentation tests.

and unloading curves show variations in maximum depth of penetration size, in the as-welded HAZ are easily observed. After creep testing,
in each region, which indicates that large variations of deformation resis- black dots of creep cavities are observed on the outer edge of the HAZ
tance exist in these regions, which is caused by the highly-heterogeneous in Fig. 6c. It is evident that cavities were present in the FGHAZ, ICHAZ,
structures right after welding thermal cycles studied in a previous work and over-tempered base metal, but the ICHAZ has the highest number
[33]. The fusion zone (FZ) exhibits the lowest displacement and the density of cavities. To examine structural evolutions across the welds,
ICHAZ shows the largest displacement in all testing stages. The FZ has EBSD analyses were conducted on the PWHT-ed and crept specimens.
the highest hardness of 5.4 GPa, and the ICHAZ exhibits the lowest hard- Characterization of the as-welded specimen was reported in a previous
ness of 1.4 GPa. Considering the creep rate shown in Fig. 5b, the ICHAZ work [33]. The PWHT is normally used to reduce hardness differences
experienced the highest deformation rate of 174.6 μm/h. Low creep between the FZ, HAZ, and base metal, and improve toughness of
strength of those over-tempered martensite probably leads to this ex- welds by homogenizing large structural variations across the welds
tremely high deformation rate in the as-welded ICHAZ. The FZ and BM [27,37]. Microstructure evolutions across the weld after PWHT
have the lowest creep rate of about 28 μm/h. In the PWHT condition (760 °C-2 h) were characterized by EBSD, shown in Fig. 7. It is notable
(Fig. 4c), no significant difference in the maximum depth of penetration that there are still large structure variations even after PWHT. The FZ
is observed, which implies that all regions have similar strength levels. still keeps the as-welded microstructure of large PAGs with wide mar-
Both the hardness (2.2–2.6 GPa) and creep rate (39–46 μm/h) for each tensite laths. Due to substructures of martensite packet and blocks, the
region are quite close, which indicates that the PWHT tempering effect measured crystal grain size of the FZ is only about 1.80 ± 1.71 μm.
is sufficient for hardness homogenization. In the crept condition The CGHAZ in Fig. 7b also shows a coarse-grained structure (average
(Fig. 4d), the variation in maximum depth of penetration is significant, size: 2.10 ± 2.56 μm). The fractions of HAGBs in both FZ and CGHAZ
which means the creep resistance between these regions varies. The FZ are about 35%. Both FGHAZ and ICHAZ in Fig. 7c and d exhibit fine-
is still the hardest region and the ICHAZ is the softest region (2.1 GPa). grained structure features. The fine grains (average size: 1.79 ±
The higher hardness values after creep test than that in the PWHT condi- 1.87 μm) in the FGHAZ is due to insufficient grain growth of austenite
tion is likely caused by the accumulated creep strain in the HAZ regions. at low peak temperatures. However, the fine grains (average size:
Locally the matrix grains were deformed after creep test and the inden- 1.95 ± 1.73 μm) in the ICHAZ are over-tempered martensite grains
tation test is very sensitive to microstructure variations. The hardness from the base metal and small transformed PAGs. The finer grain size at-
distribution trend across these tested regions is consistent with the tributed to the higher fractions of HAGBs in the FGHAZ (40%) and ICHAZ
other two conditions. For the deformation rate, the ICHAZ still has the (37%). Base metal (average size: 2.00 ± 1.53 μm) in Fig. 7e shows a
highest value of 24 μm/h, which implies its lowest strength. structure of fine equiaxed grains and tempered martensite, which has
the highest fraction (44%) of HAGBs. The kernel average misorientation
3.3. Microstructural evolutions after PWHT and creep testing (KAM) calculated from the EBSD data measures local plastic strain of
grains due to local variations in lattice orientation, which is a sensitive
Optical macrographs of the HAZ specimens under three thermal indicator of the internal dislocation density of grains. The high KAM
stages are presented in Fig. 6. Structural variations, especially PAG value indicates a high dislocation density in the structure, for example,

Fig. 6. Optical images of the welds under three thermal stages: (a) As-welded condition [31]; (b) After PWHT; (c) after creep testing.
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; 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. (b) CGHAZ; (c) FGHAZ; (d) ICHAZ; (e) BM.

un-tempered martensite. The KAM maps across the FZ to the BM are of the FZ and CGHAZ are 1.06° and 1.10°, respectively. The FGHAZ,
shown in Fig. 8. Statistical distribution of the KAM values is plotted in ICHAZ, and BM exhibit comparable distributions with normalized
Fig. 11a. It clearly shows that the FZ and CGHAZ establish higher strain KAM values of 0.95°, 0.98°, and 0.84°, respectively. These results imply
levels with more green-color regions. The misorientation peaks shift that the tempering at 760 °C for 2 h has a significant tempering effect
from 0.65° to 0.45° from the FZ to the BM. The normalized KAM values on the weld by eliminating excessive dislocations from martensitic

Fig. 8. EBSD kernel average misorientation maps of sub-regions across the weld after Fig. 10. EBSD kernel average misorientation maps of sub-regions across the weld after
PWHT: (a) FZ; (b) CGHAZ; (c) FGHAZ; (d) ICHAZ; (e) BM. 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 The FZ and CGHAZ still exhibit a structure of martensite laths. Fine
at 786 °C, an additional tempering from the PWHT further reduced the equiaxed grains are also observed in both the FZ and CGHAZ. The FZ
dislocation density of over-tempered base metal. Therefore, the KAM has the finest grain size of 0.92 ± 0.83 μm. Relative coarse grain struc-
in the over-tempered BM is expected to be the lowest among the tures (about 2 μm) with a HAGB fraction of about 55.5% are observed
three FZ, HAZ, and BM. in the FGHAZ and ICHAZ. The equiaxed shape of matrix grains indicates
The weld with a Type IV cracking after creep testing is also analyzed recovery and recrystallization occurred in these regions. The KAM maps
with EBSD for comparison in Fig. 9. It is noted that the location of the an- in Fig. 10 and distribution profiles in Fig. 11b clearly show that strain en-
alyzed FGHAZ is in the transition region between the FGHAZ and ICHAZ. 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 9

FZ and CGHAZ still maintain the highest strain levels with the KAM Fig. 14 shows creep cavities of the Type IV cracking in the ICHAZ. It is
peaks around 0.5°. Normalized KAM values in the FZ and CGHAZ are clear that cavities nucleated along high-angle grain boundaries, espe-
0.85° and 0.73°, respectively. The KAM peaks of the FGHAZ and ICHAZ cially triple junctions (Fig. 14c). Deformation and rotation of matrix
in Fig. 11b shrink into a low value of 0.15°. The normalized KAM values grains in Fig. 14b assisted nucleation of cavities. In Fig. 14d, it is evident
in the FGHAZ and ICHAZ are 0.29° and 0.30°, respectively. It should be that the cavities are always associated with coarse precipitates along
noted that the high KAM region in the FGHAZ is associated with a grain boundaries. The nucleated cavities tend to connect with each
creep cavity, which implies that large local deformation occurred during other and isolate the central grain from other neighboring grains.
cavitation. Based on the low KAM values, the FGHAZ and ICHAZ experi- These coarsened precipitates have been identified as the Cr-rich M23C6
enced a significant creep strength degradation during creep testing. carbides or Laves phases [18]. Besides the feature above, one more inter-
Combined with the indentation results in Fig. 4, the ICHAZ has the larg- esting observation is that there is always one grain which is surrounded
est deformation and the highest strain energy reduction during creep by cavities, experienced a significant deformation, but the neighboring
testing, which is considered to be the most susceptible region for the grains seems to be stronger and didn't deform much. It is believed
Type IV cracking. 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
3.4. Cavitation in the Type IV cracking 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-
The Type IV cracking was considered as a brittle fracture in terms of gion with cavities, were analyzed for comparison with the auger elec-
the low total creep strain across the gauge length, however, recent re- tron spectroscopy mapping in Fig. 15. It shows that in the cavity-free
search reported that locally it is a ductile fracture within the HAZ region, C-rich spots in Fig. 15b are correlated with the carbides observed
[38–40]. Fig. 12 shows a typical fracture surface of the specimen with in Fig. 15a. Since the nominal C composition of Grade 91 steel is low and
a Type IV cracking. Shallow dimples in Fig. 12b indicate increased only 0.11 wt%, precipitation of these coarsened carbides have consumed
creep rate (deformation) in the tertiary stage of creep testing. Some most of the C, which is one of the most efficient interstitial strengthen-
large particles, very likely inclusions, are observed inside dimples. The ing elements in the matrix. The reduced carbon lowered creep resis-
EDS maps in Fig. 13 presents distribution of the major alloying elements tance of the matrix grains during creep. High Cr spots are observed in
around a dimple. A large amount of Cr-Mo-rich spots are observed on Fig. 15c, which is likely the Cr-rich M23C6 carbides. The Cr distribution
the dimple wall, which are likely the Cr-rich M23C6 carbides. These dim- inside matrix grains is quite homogeneous, which indicates that matrix
ple wall carbides indicate there are large local deformation along grain grains have a comparable strength and would respond similarly without
boundaries during fracture. preferential deformation of individual grains. However, the situation in

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.
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 indentation test. For example, a large indentation spacing (N150 μm)
distribution. After a long-term creep test, the distribution of C is highly with a high loading force (1 kgf) in regular hardness tests only can
inhomogeneous. Carbon concentrated in certain points which correlate cover only a few measurements across the entire HAZ (2–3 mm thick-
to those coarsened carbides and microcracks. The C concentration in the ness). Since the transition region between FGHAZ and ICHAZ is
matrix itself is low close to the cavity areas. The Cr distribution in b100 μm, the large indentation spacing may easily skip this region. The
Fig. 16c is inhomogeneous inside matrix grains. This Cr concentration instrumented indentation test can have a quite small indentation spacing
difference between grains can be 2%, which causes strength mismatch (b50 μm), which can give more data points within the same region. An-
between matrix grains. Thus, during creep testing, some weak grains other advantage of the instrumented indentation is that it can give not
with low Cr concentrations preferentially deformed first, but those only hardness values, but also deformation data of each point, which
stronger ones with higher Cr concentrations deformed less. These can be used for micro-mechanics calculations, such as deformation rate.
creep deformation variations among matrix grains eventually cause In this work, by using these high-resolution tools, the most Type IV crack-
local stress concentrations and enhance nucleation of cavities as ing susceptible region has been confidently traced back to the ICHAZ.
shown in Fig. 16a. The next question to be answered is why cavities preferentially nu-
cleated in the ICHAZ. From the stress constraint perspective, it has been
4. Discussion reported that the ICHAZ experienced the largest stress triaxiality factor
[7,11]. From the microstructure point of view, formation of cracks is a
It is well-known that grain size is one of the most important traces for process of accumulating creep cavities. Growing and inter-connection
identifying the different sub-regions within the HAZ. However, the fine- of nucleated creep cavities lead to formation of microcracks. Therefore,
grained structure in both the FGHAZ and ICHAZ makes it difficult for op- the relation between stress triaxiality distribution and nucleation of
tical observations. The high-resolution FESEM images in Fig. 3 success- creep cavities may be worthy of checking. It has been reported that
fully capture the characteristic structure of fine untransformed over- the nucleation and growth of creep cavities is the dominating reason
tempered martensite in the as-welded ICHAZ. The BSE FESEM images for creep strength degradation [5,6]. To investigate nucleation of cavities
in Fig. 3 also give chemical composition contrast of the structure, which in a micro-scale level, a microstructure-based model was built and
is important to distinguish the FGHAZ and ICHAZ as well. For example, shown in Fig. 17. This simplified model contains three main structural
undissolved Cr-rich M23C6 carbide is a signature of the ICHAZ and the components, the precipitates (only M23C6) in Fig. 17b, the hard grains
BSE image in Fig. 3 clearly shows this feature, which cannot be resolved (Fig. 17c) which represent the Cr-rich grains observed in Fig. 15, and
by optical observations. The instrumented indentation test used in this the soft grains (Fig. 17d) which represents the Cr-depleted grains ob-
work overcomes some limitations of the conventional hardness served in Fig. 15. Finite element analysis was conducted with a pressure

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.
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 points close to precipitates show high stress triaxiality. Fig. 19 shows
Mises stress, and stress triaxiality are presented in Fig. 18. Generally, an example of stress triaxiality distribution in the microstructure-
similar distributions of von Mises stress and first principal stress are ob- based model and an observed creep cavity in the ICHAZ. It is obvious
served in the structure. The first principal stress level is higher than the that the coarse precipitate near the triple point of high-angle grain
von Mises stress. Local stress concentration as high as 200 MPa is ob- boundaries causes a high stress triaxiality in the triple point. A region
served to be associated with precipitates. A higher stress level with a high stress triaxiality value is also observed at the interface be-
(N70 MPa) exists in some of precipitates and adjacent regions. High tween precipitate and matrix grain. A small cavity nucleated at the
stress levels (N100 MPa) are also observed in some triple points of end of the rod-like precipitates. Grain boundary folded at triple points
grain boundaries which are high-angle grain boundaries. Fig. 18d promotes nucleation of creep cavities. Therefore, locations with high
shows the stress triaxiality distribution in the structure. Points with a stress triaxiality are likely sites for cavity nucleation.
stress triaxiality as high as 7 are observed. Their locations are different Fig. 20 schematically summaries structural evolutions in the ICHAZ
from the points with high stress levels. Some grain boundary triple 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- the FGHAZ and ICHAZ is the direct cause for the creep strength
neous Cr distribution in the as-received base metal, which causes non- degradation. Local deformation of matrix grains promotes nucle-
uniform chemical potentials of austenization. Under the rapid heating ation and growth of creep cavities. Cr inhomogeneity leads to a
thermal cycle of arc welding, heterogeneous martensite/ferrite-to- strength mismatch between those grown matrix grains during
austenite transformation occurred in the ICHAZ, which leads to the creep, which accelerates local deformation and cavity nucleation.
mixed structure of transformed martensite and untransformed but Partial dissolution of M23C6 carbides with insufficient diffusion in
over-tempered martensite. The insufficient growth of transformed aus- the ICHAZ during rapid welding thermal cycles is the main cause
tenite due to the relatively low peak temperature in the ICHAZ led to a for this alloying inhomogeneity.
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 CRediT authorship contribution statement
Grade 91 steel play a significant role in maintaining its high creep
strength. Wherever, the fine PAG size also affects the crystallographic Yiyu Wang: Conceptualization, Data curation, Formal analysis, In-
feature of martensitic transformation during cooling. It is observed vestigation, Methodology, Writing - original draft, Writing - review &
that the number of transformed martensite packets was reduced editing. Rangasayee Kannan: Formal analysis, Investigation, Writing -
when the PAG size is below 10 μm [41]. The micrograph in Fig. 2 clearly review & editing. Leijun Li: Conceptualization, Formal analysis, Writing
shows that the majority of PAGs is b10 μm. Based on the crystallography - review & editing, Funding acquisition, Supervision.
in lath martensite, the decreased packet boundaries results in a lower
number of block boundaries. Due to the limited available packet/block Declaration of competing interest
boundaries, M23C6 carbides had to nucleate and gather along the PAGs
instead of a homogeneous distribution. These decreased boundary The authors declare that they have no known competing financial
strengthening and precipitation strengthening directly lower the interests or personal relationships that could have appeared to influ-
ICHAZ's creep resistance. Meanwhile, the dissolution of Cr- rich M23C6 ence the work reported in this paper.
carbides enhanced the local Cr inhomogeneity in the ICHAZ, as shown
in Fig. 3. The transformed martensite experienced recovery of excessive Acknowledgment
dislocations generated during martensitic transformation. Whereas,
those over-tempered martensite experienced extensive recovery and This research work was sponsored by the Natural Sciences and Engi-
grain growth since they already underwent the initial recovery process neering Research Council of Canada through a Discovery Grant
as the base metal, which led to an increase of high-angle grain bound- (RES0020431). The author would like to thank Dr. Andrew Deceuster,
aries. The grain boundary migration during grain growth also pushed Dr. Bishal Silwal, and Benjamin Griffiths from the Utah State University
those undissolved but coarsened carbides to the HAGBs. These two dif- are thanked for their help on welding and creep testing experiments. Dr.
ferent evolution paths in matrix grains differentiate their strain energies Shihong Xu and Dr. Meisam Nouri from the University of Alberta are
with a heterogeneous grain growth (Fig. 20c). The EBSD KAM in Fig. 8d thanked for their help on AES and indentation tests.
roughly shows two levels of strain energies in the PWHT-ed ICHAZ. In
creep testing, the strength mismatch caused by the inhomogeneous Cr References
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