Journal of Materials Processing Tech.

266 (2019) 140–154

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Journal of Materials Processing Tech.

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

Effect of post weld heat treatments on microstructure evolution and type IV T

cracking behavior of the P91 steel welds joint
⁎
Chandan Pandeya, , M.M. Mahapatrab, Pradeep Kumarc, S. Kumara, Sachin Sirohia
a
Department of Mechanical Engineering, SRM IST Delhi NCR Campus Modinagar, Uttarpradesh, 201204, India
b
School of Mechanical Sciences, Indian Institute of Technology, Bhubaneswar, Odisha, 751013, India
c
Department of Mechanical and Industrial Engineering, Indian Institute of Technology Roorkee, Uttrakhand, 247667, India

A R T I C LE I N FO A B S T R A C T

Associate Editor Gary J Cheng The creep tests were conducted on multi-pass shielded metal arc welded P91 steel weld joint at creep exposure
Keywords: temperature of 620 °C for an applied stress of 150 and 200 MPa in as-welded, and post weld heat treatments
P91 steel (PWHTs) state. The PWHTs involved the tempering at 760 °C/2 h/air cooling (referred as PWHT) and re-aus-
Type IV cracking tenitizing at 1040 °C/60 min/air cooling + tempering at 760 °C/2 h/air cooling (refereed as PWNT). Results
Creep indicate a great influence of heat treatment conditions on the creep rupture life, fracture location and micro-
Weld joint structure evolution of the P91 welded joint. As-welded and PWHT specimens showed the Type IV mode of failure
PWNT and the fracture occurred in soft fine-grained heat affected zone/inter-critical heat affected zone (FGHAZ/IC-
PWHT
HAZ). In PWNT specimens, a shift in fracture location was observed from FGHAZ/ICHAZ to over tempered base
zone. The degree of heterogeneity in terms of the microstructure and mechanical properties across the welded
joints before the creep exposure have observed a great influence on the creep rupture life. As compared to other
heat treated specimen, PWNT specimen exhibited higher creep rupture life at the lower applied stress of 150 MPa
and creep exposure temperature of 620 °C due to lower degree of heterogeneity across the welded joints.
However, Laves phase formation (Fe2W/Fe2Mo) was noticed in different zones (weld zone + heat affected
zones) of the crept specimen for PWNT condition exposed at 620 °C for 150 MPa.

1. Introduction achieve adequate mechanical properties in the weld heat affected zones
(HAZs). The CSEF steels are differentiated on the basis of the chemical
Cr-Mo steels are used in high temperature and pressure applications composition. In recent days, it has been observed that 9% chromium
that include critical components of modern supercritical and ultra-su- together with Mo, W, V, Nb and other alloying elements provide the
percritical thermal power plants. Due to the unique ability to with- requisite mechanical and metallurgical properties to withstand high
standing high temperatures and pressure these steels are also used in operating temperature and pressure exceeding 600 °C and 300 bar, re-
critical components of fast breeder nuclear reactors. Pandey et al. spectively. Most of the thermal power plants in India utilize technology
(2016) reported that Cr-Mo steels are heat treatable and require specific resulting in a low thermal efficiency and increased emission of CO2, CO,
regimes of heat treatment to attain optimum material characteristic NOx, SO2, and particulates. The modern supercritical and ultra-super-
such as hardness, Charpy toughness, corrosion resistance, creep critical power plants operate more efficiently by accessing the elevated
strength, and tensile strength. Klueh (2005) reported the other superior operating conditions. This makes the modern power plants more eco-
properties of the Cr-Mo steels like high oxidation resistance, high-stress friendly and cost-effective. Hence, efforts are being made to structurally
corrosion cracking resistance, and adequate fracture toughness. Yan upgrade the existing power units to access the supercritical/ultra-su-
et al. (2013) reported that the metallurgical structure of Cr-Mo steels percritical operating conditions. Swindeman et al. (2004) reported that
demand strict adherence to appropriate welding procedure to get ac- for super critical/ultra-supercritical power plant, operating tempera-
ceptable weld quality characteristics such as adequate weld strength, ture and pressure exceeds 600 °C and 300 bar, respectively.
impact toughness, and creep strength. Pandey et al. (2018a) reported It is known that a typical weldments can be differentiated in three
that the solidification of Cr-Mo steel leads to the formation of marten- different zones, the weld fusion zone, HAZ and the over tempered base
sitic microstructure which necessitates further heat treatment to metal exhibiting distinct topology of microstructure and mechanical

⁎
Corresponding author.
E-mail addresses: [email protected], [email protected], [email protected] (C. Pandey).

https://doi.org/10.1016/j.jmatprotec.2018.10.024
Received 17 February 2018; Received in revised form 3 October 2018; Accepted 20 October 2018
Available online 25 October 2018
0924-0136/ © 2018 Elsevier B.V. All rights reserved.
C. Pandey et al. Journal of Materials Processing Tech. 266 (2019) 140–154

properties. The microstructure of the weld is mostly analogous to the et al. (2017) studied the evolution of Laves phase in modified 9Cr-1Mo
dendritic microstructure of a miniaturized cast of an alloy. However, steel and their influence on creep rupture behaviour. These inter-
the same cannot be said for the heat affected zone. It is observed in most metallic compounds coarsen with time leading to creep cavity forma-
of the weld failure that, the defect is initiated in the soft HAZ. Silwal tion and limit the rupture life of the components. Furthermore, as the
et al. (2013) reported that the HAZ of the weld content distinct zones of P91 weld fusion zone microstructure differs from that of HAZ and base
the microstructure with varying mechanical properties and grain sizes. metal, different effects of creep exposure on rupture life of the welded
The variation of the mechanical properties such as toughness and joint are observed with respect to its different macrostructure zones.
hardness across HAZs can be high which might lead to the initiation of Hence, it is extremely important to determine the safe creep exposure
the defects in the weakest zone. Such variation of microstructural and temperature.
mechanical properties in HAZs can be very severe in high strength steel In the present work, the effect of creep exposure temperature and
such as Cr-Mo steels. The HAZs of Cr-Mo steel weld (such as P91) is applied stress on the rupture behavior and microstructure evolution of
martensitic with varying hardness and Charpy toughness. Francis et al. the Cr-Mo P91 welds have been studied in detail. The effect of heat
(2006) reported that the weakest among the three zones is known as the treatments on fracture location and Type IV cracking behavior of the
inter critical heat affected zone (ICHAZ) which is highly susceptible to P91 steel weld joint has also been presented.
Type IV cracking during the creep exposure. Akram et al. (2018) had
also reported the formation of soft zone in ICHAZ for dissimilar weld 2. Experimental details
joint of P91/Ni alloy. Hence, homogeneous microstructure across the
weldments is primary requirement of the welded joint to achieve the 2.1. Material, groove preparation, and welding
higher creep rupture life. Consequently, Cr-Mo P91 welds are subjected
to post weld heat treatment (PWHT) to attain desirable microstructure The plate of dimension 150 mm (length) × 90 mm(width) × 18 mm
and mechanical properties. That results in inferior creep properties of (thickness) was machined from cast and forged P91 steel plate for the
the weld joints as compared to both the base metal and the weld metal. weld joint preparation. The groove was designed with a bevel angle and
Akram et al. (2017) studied the creep rupture behaviour of the dis- root face height of 37.5°, 1.5 mm, respectively. The root gap was
similar P91 and AISI304 weld joint using different layer of Inconel. The maintained 1.5 mm. The tacking of plates was carried out to overcome
stress component of 3 was reported using threshold stress concept that the distortion. The root pass was prepared with AWS ER90S-B9
deals with the creep deformation to be viscous glide as a result of solute (9CrMoV-N) filler using (φ1.6 mm, cut length 1000 mm) using gas
drag. They had also analyzed the creep data using the Monkman-Grant tungsten arc welding (GTAW) process. The filling pass was performed
relationship and creep damage tolerance factor (λ). Wang et al. (2018) using the welding consumable rod (AWS E9015-B9) of diameter 4 mm
reported that the ICHAZ experiences a temperature between Ac1 and with shielded metal arc welding (SMAW) process. Table 2 indicated the
Ac3, while fine-grained heat affected zone (FGHAZ) temperature is just welding process parameters used for the root pass and filling passes. All
above the Ac3. Abson and Rothwell (2013) reported that the soft FGHAZ steps starting from the groove preparation to completion of welding
and ICHAZ location served as the most preferential location of the Type include tacking of plate, root pass, filling pass, and removal of tacking is
IV cracking. Both FGHAZ and ICHAZ possesses the fine grain structure discussed in my earlier work (Pandey et al., 2017b). Table 1 shows the
with partially dissolved M23C6 precipitates and make it difficult to chemical composition of the base metal, GTAW filler wire and SMAW
distinguish after the PWHT. In coarse grain heat affected zone high- filler rod.
temperature results in complete dissolution of these precipitates and
lead to the formation of the microstructure similar to the normalized 2.2. Heat treatment of the welded joints
P91 steel. The different zone of P91 steel show different response to the
tempering treatment. Pandey and Mahapatra (2016) reported that After the welding, the joints were subjected to two different heat
minimum hardness exists in the ICHAZ even after the PWHT. Pandey treatments. In 1st condition, the welded plates were allowed to cool in
et al. (2018b, 2018c) reported that re-austenitizing based tempering the air just after the welding (Table 3). In other two cases, the welded
(PWNT) of the welded joints produced uniform microstructure and plates were subjected to the post weld heat treatments (PWHTs) as per
hardness across the weld joints. In PWNT, welded sample heated in the Table 3.
normalizing temperature range and after that tempered in the tem-
perature range of 730–760 °C for 2 h. A superior microstructure and 2.3. Creep tests and microstructural study
mechanical properties in PWNT condition is also reported by the
Manugula et al. (2017). For P91 steel, the manufacturer generally de- For creep tests, creep test specimens were machined from the
scribe a range of safe operating temperature. The operating range may welded plate with gauge diameter and gauge length of 4 mm and
be narrow which demands accurate control of the operating tempera- 50 mm, respectively. The weld joint was in the center of the specimen.
ture as slight variation might lead to severe deterioration in the creep The. Creep tests were conducted at fixed temperature of 620 °C for low
strength. At lower range of operating temperature, the creep strength stress (150 MPa) and high applied stress (200 MPa) as per Table 4.
remains mostly unaffected. However, beyond a particular temperature The microstructure of the various zones of the crept specimen was
limit the detrimental intermetallic phases (such as Laves and Z-phase) examined using the scanning electron microscope (SEM) and optical
are formed. Danielsen et al. (2013) reported the evolution of inter- microscope after etching with Vilella’s reagent. The microstructures
metallic Z-phase and their crystal structure in 9–12 % Cr steels. Zhang were taken before and after the creep rupture test in different heat

Table 1
Chemical composition of P91 steel plate, SMAW filler rod and GTAW filler wire, wt.%.
Element Chemical composition, wt%

C Cr Mo V Ni Si Mn Nb N S

P91 steel 0.10 8.16 0.71 0.18 0.30 0.19 0.67 0.05 < 0.02 0.02
SMAW filler rod 0.08–0.12 8–10 0.85–1.1 0.15–0.30 0.4–1.0 0.20-0.50 0.40-1.00 0.04–0.08 0.03-0.07 max
0.02
GTAW filler wire 0.12 9.0 0.90 0.20 0.50 0.30 0.50 0.06 < 0.02 0.02

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Table 2 size less than 40 nm are V and Nb-rich MX type carbide and carboni-
Details of the welding process parameters. trides precipitates (Panait et al., 2010). The density of the precipitates is
Passes Welding Welding Arc voltage Travel speed observed to be higher along the lath blocks as compared to the intra-
process current (amps) (V) (mm/sec) lath region.

Root pass (1, 2) GTAW 110–120 14–16 2.14

Filling passes SMAW 140–151 21–25.6 3.20–5.36
3.2. Creep tests
(14)

3.2.1. Creep deformation and rupture behavior of weld joints

Table 3 Fig. 2 shows the creep ruptured specimen. Table 5 indicated the
Heat treatment regime performed on the welded joint. creep ruptured life and minimum creep rate for the different creep test
conditions. The creep ruptured life was measured 100 h and 1002 h for
Welded joint Heat treatments
as-welded 1(200 MPa) and as-welded 2 (150 MPa) condition, respec-
Normalizing Tempering tively. For high applied stress (as-welded 1) fracture was noticed in over
tempered base zone and referred as Type V crack (Yamazaki et al.,
st
1 (As-welded) – – 2007). In as-welded 2 condition, typical Type IV cracking is observed
2nd (PWHT) – 760 °C for 2 h, followed by
and fracture occurs form the soft FGHAZ. In PWHT condition, Type IV
air cooling
3rd (PWNT) re-austenitizing at 1040 °C for 760 °C for 2 h, followed by cracking is noticed for both low and high appplied stress, as shown in
60 min/air cooling air cooling Fig. 2. PWHT of welded joint results in a significant increase in creep
rupture life as compared to as-welded condition for the high level of
applied stress of 200 MPa (PWHT 1). The creep rupture life increased
Table 4 form 100 h to 322 h. However, for PWHT 2 condition poor creep rup-
Creep tests condition. ture life is observed as compared to as-welded 2 condition and it de-
S. No. Creep test condition Temperature (oC) Applied stress (MPa) creased from 1002 h to 350 h. In PWNT condition, the uniform micro-
structure and hardness were reported across the welded joint of P91
1 As-welded 1 620 200 steel. For PWNT 1, the creep rupture life was measured 466 h which
2 As-welded 2 150
was higher than the as-welded 1 and PWHT 1 condition. In PWNT 1
3 PWHT 1 200
4 PWHT 2 150 state, creep rupture life was measured 44.72% higher than PWHT 1 and
5 PWNT 1 200 33.14% higher than PWHT 2 condition. Maximum creep rupture life of
6 PWNT 2 150 2432 h was measured for the PWNT 2 and it was 594.895% higher than
PWHT 2 condition and 142.7% higher than as-welded 2 conditions.
After the PWNT treatment, the fracture location was also shifted form
treatment condition. The microhardness measurement across the the soft FGHAZ (Type IV) to over tempered base zone (Type V) due to
weldments in different crept condition were taken using the Vickers homogeneity across the weldments. To locate the fracture location,
microhardness tester (Omnitech S. auto) at a load of 500 g for 10 s of macrostructure is shown in Fig. 2.
dwell time. The creep curves of P91 weld joints under different operating con-
ditions and corresponding to different applied temperature and stress
3. Results and discussion are shown in Fig. 3(a–b). Typical creep curve for PWHT 1 condition is
depicted in Fig. 3(c). The creep curve exhibits small instantaneous
3.1. As-received material strain on loading, a transient primary stage, secondary steady-stage and
prolonged accelerating ternary stage. It is difficult to distinguish the
Typical micrograph of as-received P91 steel is shown in Fig. 1. The primary creep stage for the lower level of applied stress (150 MPa), as
optical micrograph shows the different orientation of lath blocks inside shown for PWNT 2 and PWHT 2. Longer secondary creep stage is
the lath packets (Fig. 1(a)). The higher accumulation of precipitates is clearly observed for the lower level of applied stress at 620 °C of creep
observed along the lath blocks in black dotted form. Fig. 1(b) shows the exposure (PWNT 2 and PWHT 2). A longer secondary creep stage is also
morphology and distribution of the precipitates along the lath bound- observed for PWNT 1 condition. For applied stress of 200 MPa, max-
aries and in matrix region. Along the lath blocks, uniform distribution imum percentage elongation is observed for PWHT 1 and minimum for
of globular and spherical shape precipitates are observed while inside as-welded 1. In thelow level of applied stress (150 MPa) for same creep
the matrix region fine spherical precipitates are observed. Pandey et al. exposure temperature, PWNT 2 condition produces the maximum
(2017) reported that the particles having a size in the range of elongation. The minimum creep rate variation with applied stress is
100–240 nm are mainly Cr, W, and Mo-rich M23C6 while particles of given in Fig. 3(d). The minimum creep rate increases with increase in

Fig. 1. Typical optical micrograph and SEM image of cast and forged P91 steel plate (a) and (b), respectively.

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Fig. 2. Fractured creep tested specimen with fracture location and creep exposure time (Pandey et al., 2018a).

Table 5 the applied stress. The value n = 3 is taken for the Solute-drag creep
Creep test results. where the rate of migration of solute atoms control the moving dis-
Creep test Creep exposure Min creep rate Fracture
locations. In case of a dislocation climb controlled process, the value of
condition time (h) (h−1) location stress component (n) = 5. Sherby and Taleff(2002) stated that the
dislocation climb controlled mechanism occurred in the materials
As-welded 1 100 ± 5 2.30 × 10−2 BM which showed sub-grain formation and power-law breakdown (PLB)
As-welded 2 1002 ± 10 8.71 × 10−4 FGHAZ
PWHT 1 322 ± 8 9.16 × 10−3 FGHAZ
behavior. The stress component is considered as 8 for the dislocation
PWHT 2 350 ± 8 5.88 × 10−3 FGHAZ climb controlled mechanism in which microstructure remain constant
PWNT 1 466 ± 10 3.66 × 10−3 BM during the creep exposure. In the present investigation, the n value of
PWNT 2 2432 ± 15 6.79 × 10−4 BM 11, 2 and 6 have been observed for as-welded, PWHT and PWNT
condition. The lowering in n value is observed mainly due to excessive
microstructure change at high temperatures such precipitate coar-
applied stress, as shown in Table 5. The minimum creep rate (εs ) var-
sening, Laves phase formation and a decrease in coherent strain be-
iation with applied stress followed Norton’s power law of creep
tween the matrix and MX precipitates. Abe (2001) also reported the
(εmin = Aσ n ). For Harper-Dorn creep, stress component (n) = 1 is con-
similar results.
sidered. In Harper-Dorn creep, the dislocation density is invariant with

Fig. 3. (a)Creep curves for as-welded, PWHT and PWNT condition at (a) 620 °C/200 MPa, (b) 620 °C/150 MPa, (c) creep curves at a temperature of 620 °C and a
stress of 200 MPa (PWHT 1) with the three dominant stages (Transient, steady, and accelerated stage), (d) stress dependence of minimum creep rate at 620 °C.

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Fig. 4. Variation in creep rate as a function of creep exposure time and heat treatment condition (a) as-welded 1, (b) PWHT 1, (c) PWNT 1, (d) as-welded 2, (e) PWHT
2, (f) PWNT 2.

Table 6 3.3. Microstructure evolution in as-welded and PWHTs condition

Reduction in area (%) and elongation (%) for different creep test conditions.
Creep test condition Reduction in area (%) Fracture elongation (%)
Pandey et al. (2017b) have discussed in details about the micro-
structure of the different zone including weld fusion zone (WFZ), HAZs
As-welded 1 91 7.16 (CGHAZ, FGHAZ and ICHAZ) in P91 welded plate. In as-welded con-
As-welded 2 94 6.50 dition, the microstructure of the WFZ shows the typical columnar laths
PWHT 1 92 9.38
with negligible precipitates, as shown in Fig. 5(a). The complete dis-
PWHT 2 94 7.50
PWNT 1 83 7.20 solution of the precipitates lead the higher C and N percentage in the
PWNT 2 89 14.43 solution matrix and results in brittle microstructure. In FGHAZ, partial
dissolution of the precipitates results in heterogeneous microstructure
formation. The coarse precipitates remain undissolved and provide the
For different creep exposure condition, the variation of strain rate pinning effect to the prior austenite grain boundaries (PAGBs) and lead
with creep exposure time is shown in Fig. 4(a–f). The pronounced to the formation of the fine grain structure. In FGHAZ, both equiaxed
ternary stage of creep deformation is clearly observed in Fig. 4. In and columnar laths are formed, as shown in Fig. 5(b). In ICHAZ,
primary stage of creep regime, creep rate decreases significantly with equiaxed tempered laths are formed with partial tempering and coar-
creep exposure time and followed by the region of minimum creep rate. sening of the precipitates. The tempering and coarsening of the pre-
After the steady-state creep stage, faster rate of creep deformation is cipitates result in poor hardness and higher ductility of the ICHAZ
observed in tertiary stage till the fracture of the specimen. The P91 among HAZs (Pandey et al., 2017a). The coarse precipitates are clearly
welded joints spent the majority of rupture time in the tertiary stage for shown in Fig. 5(c). Hence, in as-welded condition, different zones show
each condition except the PWNT 2 condition. In primary transient creep the different microstructure and mechanical properties that result in
stage, the decrease in strain rate is attributed to the work hardening heterogeneous microstructure formation across the welds joint.
behavior of material as a result of multiplication and interaction of the To overcome the heterogeneity across the welds joint, PWHT was
dislocations. After the certain period of the time, work hardening and performed. Typical micrograph of the different zone after the PWHT is
recovery mechanism reach to the equilibrium state and leads to con- shown in Fig. 5(d–f). The columnar lath morphology still remains in the
stant strain rate due to dislocation annihilation and rearrangement. weld fusion zone. However, the lath boundaries get decorated with the
Sakthivel et al. (2015) reported that in the last stage, coarsening of precipitates, as shown in Fig. 5(e). The FGHAZ and ICHAZ look similar
precipitates and growing creep cavities accelerate the creep rate. The after the PWHT and shows the formation of tempered lath martensite
minimum strain rate is observed to be increased with increase in ap- with blocks and packets. The lath blocks and packets are decorated with
plied stress for each condition, as given in Table 5. The elongation to the coarse and fine precipitates that are confirmed as M23C6 and MX
failure and reduction in area for each case is depicted in Table 6. The precipitates, respectively. The micrograph of FGHAZ and IC-HAZ is
creep specimens are fractured in a ductile manner with external shown in Fig. 5(e) and (f), respectively. The microstructure in the
necking. In as-welded and PWHT condition, the % reduction in the area different zone still shows the different microstructure however het-
is measured more than 90%. In PWNT 1 and PWNT 2 condition, the erogeneity is observed to be reduced as a result of the PWHT. The
percentage reduction in area is measured to be 83.47% and 88.6% re- micrograph in PWNT condition is shown in Fig. 5(g–i). The re-auste-
spectively. The percentage reduction in the area is measured o be nitizing of the welded joint results in complete untempered martensite
higher for the stress of 150 MPa as compared to 200 MPa. The % formation in each zone of the welds joints and it behave as the nor-
elongation is also reported in Table 6. In as-welded and PWHT condi- malized P91 steel. The normalizing results in the formation of un-
tion, percentage elongation is measured to be higher for the applied tempered lath martensite in each zone along with the complete dis-
stress of 200 MPa, but in PWNT condition, maximum percentage solution of precipitates in each zone of the weld joint. The tempering of
elongation is measured for the applied stress of 150 MPa. re-austenitized P91 welds joint leads to the formation of tempered

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Fig. 5. Typical micrograph in as-welded condition (a) weld zone, (b) FGHAZ, (c) ICHAZ; micrograph in PWHT condition (d) weld zone, (e) FGHAZ, (f) ICHAZ;
micrograph in PWNT condition (g) weld zone, (h) FGHAZ, (i) ICHAZ.

martensite in each zone and welds joint behave as the as-received P91 with fine precipitates are observed in Fig. 6(b). In PWHT 1 condition,
steel in normalized and tempered condition. The different zone shows fine precipitates are observed as compared to as-welded 1 condition. In
the equiaxed tempered lath martensite with coarse precipitates. How- PWNT 1 condition, higher density of coarse precipitates are noticed
ever, Pandey et al. (2017a) reported that size of precipitates measured along the PAGBs (Fig. 6(c)). For as-welded 2 condition, i.e. low applied
in the PWNT condition was higher than the PWHT condition that might stress of 150 MPa, microstructure looks similar to as-welded 1 condition
be the cause of inferior creep rupture strength of the welds joint after with the smaller size of precipitates. In PWHT 2 condition, micro-
the long-term creep exposure. However, PWNT results in homogeneous structure reveals the presence of coarse precipitates along with evolu-
microstructure formation along the P91 weld joint. tion of new prior austenite grains (Fig. 6(d)). The equiaxed lath mor-
phology with new subgrains are shown in Fig. 6(e). The microstructure
of PWNT 2 condition looks completely different due to the presence of
3.4. Microstructure evolution during creep exposure many coarse precipitates along the boundaries. The Laves phase for-
mation is also observed for PWNT 2 condition which is confirmed in
Fig. 6 shows the microstructure of fine grain heat affected zone in later discussion. The Laves phases are shown in Fig. 6(f). The detailed
different creep test conditions. For as-welded 1 condition, micro- phase analysis was carried out using the elemental and line mapping as
structure consists of equiaxed laths with agglomeration of precipitates discussed later.
inside the matrix region and near to PAGBs. In PWHT 1 condition, lath Fig. 7 shows the detail microstructure analysis of FGHAZ for the
blocks and PAGBs are easily traceable from the precipitates. The PAGBs

Fig. 6. Microstructure of fine-grained heat affected zone for crept specimen under different creep test condition (a) as-welded 1, (b) PWHT 1, (c) PWNT 1, (d) as-
welded 2, (e) PWHT 2, (f) PWNT 2.

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Fig. 7. Microstructure of weld fusion zone for creep exposure at 620 °C at stress of 200 MPa (as-welded 1 condition).

crept sample exposed at 620 °C for 200 MPa (as-welded 1). The coarse observed in weld fusion zone and FGHAZ are generally globular or
precipitates are observed at the lower magnification, as shown in spherical shape. The needle shape particles are observed in FGHAZ and
Fig. 7(a). The agglomeration of precipitates is observed at higher ICHAZ. The width of needle shape particles varies from 68 to 174 nm
magnification (Fig. 7(b)). A lot of fine M23C6 precipitates form a cluster with an average of 113 ± 34 nm and length from 208 to 404 nm with
and get collected around the single particles. The agglomeration is an average of 282 ± 72 nm. The size of bulky clusters are measured in
generally observed inside the matrix region. The precipitates along the range of 1132–1160 nm. The needle or chain-like shape and bulky
lath and grain boundaries do not show such type of behavior. particles are confirmed as the Laves phase. The size of Nb and V-rich
In as-welded and PWHT condition, microstructure looks similar in fine MX particles are measured in range of 20–40 nm. Hence, In PWNT
FGHAZ except for the lath morphology and agglomeration of pre- 2 condition, presence of coarse precipitates after the heat treatment
cipitates in as-welded 1 condition. The coarse precipitates of size in the leads to formation of Laves phase during the creep exposure. The detail
range of 300–400 nm are observed in PWNT 1 condition. The micro- characterization of the Laves and M23C6 phase are discussed in the next
structure of various heat affected zone and weld fusion zone for the section.
crept welded sample in PWNT 1 and PWNT 2 condition are shown in The soft FGHAZ shows further softening behaviour during the creep
Fig. 8. For PWNT 1 condition, coarse bulky precipitates are observed in exposure. The FGHAZ microstructure shows the complex mixture of
the WFZ while in HAZs the precipitate morphology looks similar. The retained base metal and newly developed microstructure. The ele-
lath morphology is clearly observed in HAZs. For PWNT 1 condition, mental mapping was performed to understand the transformation of the
the size of the cluster is measured in the range of 370–1227 nm with an microstructure during the creep exposure. The elemental distribution
average of 820 nm. In HAZs, the size of M23C6 precipitates of spherical includes the main element Cr, Fe, Mo, C, V and Nb. The as-received base
shape is measured in the range of 60–335 nm. The coarse precipitates metal and FGHAZ for as-welded 2 and PWHT 2 were examined. The
are generally observed along the PAGBs. The needle shape particles elemental mapping is shown in Fig. 9. Carbon and Chromium are the
having width varies from 68 to 127 nm with an average of 87 ± 21 nm leading alloying element in P91 steel. In Steel, diffusion of C occurs at
and length from 238 to 463 nm with an average of 327 ± 78 nm. The higher rate as compared to the subsitutional Cr. The distribution of C is
precipitates having a size in the range of 20–35 nm are also observed uniform in as-received state (Fig. 11(b1)). After creep exposure, higher
inside the matrix region which are confirmed as Nb-rich MX pre- density of C particles are observed in FGHAZ (Fig. 9(b2) and (b3)).
cipitates from the later discussion. In WFZ (Fig. 8(a)), the cluster for- Along the PAGBs and lath blocks, high intensity of C confirms the
mation might be due to the nucleation of Laves phase. For PWNT 2, the carbide precipitates. The Cr mapping shows a large scale variation for
microstructure of each zone is shown in Fig. 8(d–f). In PWNT 2 con- as-received and crept specimen, as shown in Fig. 9(c1)-11(c3). The
dition, the clustering of precipitates is observed along the PAGBs and variation in Cr distribution was noticed both at the grain level and lath
lath boundaries in each zone which are confirmed as the Laves phase. packets/blocks. The Cr concentration varies form one PAGB to other
Hence, In PWNT condition, longer creep exposure time leads to the PAGB. The higher concentration is observed for the grain at the center
formation of Laves phase in weld fusion zone and HAZs. The size of as compared to the adjacent grain, lath blocks and packet boundaries.
M23C6 precipitates is varied from the 90–285 nm. The precipitates Mo shows the uniform distribution in the matrix for the as-received

Fig. 8. Microstructure of subzones in crept specimen for PWNT 1 and PWNT 2 condition (a) and (e) weld fusion zone; (b) and (f) CGHAZ; (c) and (g) FGHAZ; (d) and
(h) ICHAZ.

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Fig. 9. Local chemistry analyses of the as-received base metal and FGHAZ for as-welded 2 and PWHT 2 condition at three thermal stages by elemental mapping of C,
Cr, Mo, Nb and Fe: (a1), (b1), (c1), (d1), (e1), (f1)-the as-received base metal; (a2), (b2), (c2), (d2), (e2), (f2)-the as-welded 2 FGHAZ; (a3), (b3), (c3), (d3), (e3), (f3)-
PWHT 2 FGHAZ; EDS spectra for (g1) as-received base metal, (g2) as-welded 2 FGHAZ, (g3) PWHT 2 FGHAZ.

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Table 7 percentage of Nb shows the formation of Nb-rich MX particles. In WFZ,

The EDS spectra of the point shown in Fig. 10. EDS spectra of point 3 confirm the formation of Cr and Mo-rich M23C6
Point No. EDX results of precipitates; element wt.% and Nb-rich MX precipitates while the EDS spectra of point 4 and 5
shows the formation of Mo-rich Laves phase (Fe2Mo) and Nb-rich NbX
C Cr Fe Mo V Nb Possible Phase (X: C, N) type carbide and carbonitrides precipitates. In other zone, the
EDS spectra show the similar results and confirm the formation of Cr-
Matrix 5 9 84 1 0.16 0.03 Cr-Mo-rich M23C6, Fe matrix
1 14 17 63 1 0.50 4 Cr-Mo-rich M23C6 rich M23C6 and Nb-rich MX precipitates. For detail investigation of the
2 13 19 62 1 0.30 4 Cr-Mo-rich M23C6 Laves phase formation in WFZ, line and elemental mapping are per-
3 7 20 62 – 0.60 10 Cr-rich M23C6, Nb-rich NbX formed, as shown in Fig. 11.
4 10 11 60 11 0.30 7 Mo-rich Laves phase, Nb-rich NbX For PWHT 2 and as-welded 2 conditions, fracture occurs from the
5 11 13 59 12 2.00 14 Mo-rich Laves phase, Nb-rich NbX
soft FGHAZ which are characterized in Fig. 11 and no any evidence of
6 19 16 55 – 0.50 9 Cr-rich M23C6, Nb-rich NbX
7 16 14 59 3 0.30 7 Cr-Mo-rich M23C6, Nb-rich NbX Laves phase formation are observed. In PWNT 1 condition, fracture
8 12 16 64 1 0.42 6 Cr-rich M23C6, Nb-rich NbX occurs from the base zone which is characterized in Fig. 10. The EDS
9 14 13 65 – 0.83 8 Cr-rich M23C6, Nb-rich NbX spectrum confirms the formation of coarse carbide precipitates in dif-
10 12 17 61 – 1.00 10 Cr-rich M23C6, Nb-rich NbX
ferent HAZs. However, the EDS spectrum of precipitates in WFZ con-
11 16 16 60 – 0.75 8 Cr-rich M23C6, Nb-rich NbX
firms the Laves phase formation and depicted in Table 7. The elements
Fe, Cr, Mo and Nb shows the homogeneous distribution in as-received
state (Fig. 9(d1)). For as-welded 2 (tr = 1002 h), the segregation of the condition as shown in Fig. 9. After the creep exposure, the accumula-
Mo particles is observed along the PAGBs. In as-welded 2, higher Mo tion of Mo and Nb took place in some specific region, as shown in
intensity spots indicates the Mo-rich carbide. In PWHT 2 condition, the Fig. 11(d). The high Mo intensity spots are related to the formation of
uniform distribution of Mo particles are observed due to poor creep Laves phase and Nb rich spot can be considered as the accumulation of
rupture life (Fig. 9(d3)). The higher Cr intensity spots confirms the fine NbX precipitates. Fig. 11(a) shows the morphology and clustering
formation of Cr-rich M23C6 precipitates. Nb particles shows the uniform behavior of the Laves phase. The size of Laves phase is higher than the
distribution within the matrix for all the three conditions (Fig. 9(e1)- M23C6 precipitates as a result of their fast growing nature. The mean
11(e3)). The Fe mapping shows the opposite trend as compared to the size of Laves phase is measured 350 nm. The line mapping of the cluster
Cr. The higher intensity spot of Cr leads to the poor intensity for the Fe. of precipitates also confirms the higher intensity of Mo and Nb peaks, as
With increase in creep exposure time, the percentage of Cr is increased shown in Fig. 11(c). That confirms the formation of NbX and Laves
in M23C6 as reported by Yan et al. (2013). The distribution of Fe is phase. Fig. 11(c) shows that at globular shape precipitates, the peak
shown in (Fig. 9(f1)-11(f3)). The EDS spectrum of the precipitates is intensity of Fe decreases and peak intensity of Cr, Mo and Nb increases.
shown in Fig. 9(g1)-11(g3). The EDS spectra confirms the formation of The EDS spectra of the matrix are shown in Fig. 11(b).
secondary phase carbide precipitates. An increase in weight percentage In PWNT 2 condition, each zone shows the accumulation of the
of Cr and Mo is observed with increase in creep exposure time from coarse precipitates along the PAGBs after the creep rupture, which is
350 h (PWHT 2) to 1002 (as-welded 2). depicted in Fig. 8(e–h). The clustering behavior of the precipitates
The EDS spectra of the precipitates form in the different zone of the along the PAGBsshows the formation of the Laves phase. In order to
crept PWNT 1 sample is given in Table 7. The points selected for the confirm the formation of the Laves phase, the different zone of the crept
EDS spectra are given in Fig. 10 and Fig. 11. PWNT 2 sample is characterized using line and elemental mapping. The
The EDS spectrum of the matrix confirms the presence of secondary weld fusion zone characterization is shown in Fig. 12. Fig. 12(a) shows
phase Cr and Mo-rich carbide precipitates along with Fe matrix. The the agglomeration of the precipitates near the Cr-rich M23C6 pre-
EDS spectrum of precipitates near the crack tip confirm the formation of cipitates. The EDS spectra of the precipitates (Fig. 12(b)) confirms
M23C6 precipitates enriched in Cr and Mo. The higher weight formation of Mo and Cr-rich M23C6, Mo-rich Laves phase and Nb-rich
MX precipitates. The line mapping shows the drastic decrease in the

Fig. 10. Microstructure of subzones in PWNT 1 condition used for the EDS spectra, (a) crack tip, (b) WFZ, (c) CGHAZ, (d) FGHAZ.

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Fig. 11. For PWNT 1 condition: (a) micrograph of weld fusion zone at 50 Kx, (b) EDS spectra of the matrix, (c) line mapping of the precipitates, (d) elemental
mapping of the precipitates.

peak intensity of Fe at globular shape coarse precipitates and same time Hence, heterogeneity in the Cr concentration leads to the hetero-
drastic increase in peak intensity of Mo and Nb, as shown in geneous microstructure and phase transformation in WFZ and HAZs.
Fig. 12(c–d). The higher intensity of Mo and Nb particles also confirm That results in the formation of the creep-susceptible region.
the formation of Laves phase in the WFZ. The elemental mapping of the For PWNT 2 condition, characterization of FGHAZ in the crept
weld fusion zone is shown in Fig. 13. The elemental mapping of the sample is shown in Fig. 14 and Fif. 15. The microstructure used in
precipitates shows the uneven distribution of the precipitates like Mo, elemental analysis and line mapping is shown in Fig. 14(a). The EDS
Cr, Fe, and Nb. The accumulation of Nb and Mo particles and dimin- spectra confirm the higher weight percentage of Mo, Nb, and Cr that
ishing of Fe particles near the precipitates confirm the Laves phase indicates the presence of Mo-rich Laves phase, Mo, Cr-rich M23C6 and
formation along with fine NbX precipitates. However, the Mo-rich Nb-rich NbX. The EDS spectrum are shown in Fig. 14(b). The line
Laves phase and Nb-rich NbX precipitates are surrounded with the Cr- mapping of the precipitates shows the higher peak intensity of Mo and
rich M23C6 precipitates. The coarsened M23C6 precipitates enriched in Nb at coarse precipitates and higher peak intensity of Cr at point 1. The
Cr are recognized in Fig. 15 by high spot intensity. The Cr-rich pre- combined elemental mapping is shown in Fig. 14(d). The elemental
cipitates along the PAGBs are always associated with the creep cavities mapping shows the higher density of Mo and Nb particles and poor
due to its brittle nature. The distribution of Cr become more nonuni- density of Fe particles at coarse bulky shape precipitates. The bulk
form in WFZ for creep tested specimen under PWNT 2 condition as deposition of Mo and Nb at bigger size precipitates confirm it as Laves
compared to as-received and PWHT 2 and as-welded 2 condition. The phases along with NbX, as shown in Fig. 14(f–g). Fig. 14(h) shows the
Cr-depleted PAGBs exhibits lower strength as compared to the PAGBS higher concentration of Cr around the bulky size particles. V shows the
with higher CR concentration. The Cr-depleted PAGBs deformation uniform distribution (Fig. 14(i)).
leads to the grain boundary sliding and creep cavities nucleation as a In PWNT 2 condition, ICHAZ of the crept sample is shown in
result of the accumulation of the vacancies. The vacancy movement is Fig. 15(a) at 50000x magnification. The EDS spectra of the bulky pre-
always associated with the shape morphology of the grain. Thus the cipitate ensure the formation of Laves phase and Nb-rich MX pre-
deformation of the matrix as a result of the applied stress leads to the cipitates (Fig. 15(b)). The line mapping also shows the drastic increase
cavity nucleation. The mismatch in the Cr concentration leads to the in the peak intensity of the Mo and Nb at the precipitates with a si-
strength variation and ultimately promotes the local deformation. multaneous decrease in the peak intensity of Fe. However, a minute

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Fig. 12. (a) Microstructure of weld fusion zone in PWNT 2 condition used for EDS spectra, line mapping and elemental mapping, (b) EDS spectrum of particle, (c) and
(d) line mapping.

Fig. 13. Elemental mapping of the weld fusion zone for PWNT 2 condition.

change is observed in the peak intensity of Cr. The elemental mapping (1995). In PWNT 2 crept sample, the clustering nature of the Laves
of the bulky precipitates shows the higher density of Mo and Nb and phase results in lath widening due to a reduction in preventing the
confirms the formation of Laves phase and NbX (Fig. 15(e) and (f)). effect of Laves phase to lath boundaries migration. In P91 steel,
However, the Fe density is negligible at the bulky precipitates. In strengthening from the Mo atoms is consider at the important
ICHAZ zone, Laves phase shows the chain like shape with bulky par- strengthening mechanism. However, the precipitation of intermetallic
ticles. Isik et al. (2014) reported the two stages of the Laves phase Laves phase is inevitable for P91 steel because Mo and W are the main
growth. At the initial stage of the nucleation, it grows into rod-like alloying element in Laves phase. Zhang et al. (2017) concluded that the
shape along the PAGBs and lath boundaries and after that, it morphs formation of Laves phase is thought to be responsible for premature
into chain-like shape and some bulky shape particles. In weld fusion failure during the creep exposure as a result of void growth.
zone, the Laves phase is observed in bulky shape while in the ICHAZ, The nucleation and growth of the Laves phase are also summarized
the chain-like shape is observed. in a schematic microstructure scenario (Fig. 16). Fig. 16(a) shows the
The evolution of Laves phase strongly affects the microstructure and preferential sites for M23C6 nucleation (micrograin boundary). The
creep behavior of the P91 steel. In P91 steel, Laves phase evolution is precursor phenomenon of the Laves phase nucleation during the creep
considered as harmful because the nucleation and growth of Laves exposure is shown in Fig. 16(b). It shows the segregation of Mo parti-
phase result in diffusion of Mo from the matrix to Laves phase and leads cles along the micrograin boundary. The Laves phase nucleation at
to weakened solution strengthening as reported by the Miyahara et al. micrograin boundary is shown in Fig. 16(c). It generally nucleates at

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Fig. 14. a) Microstructure of FGHAZ in PWNT 2 condition used for EDS spectra, line mapping and elemental mapping, (b) EDS spectra of particle, (c) line mapping;
elemental mapping (d) Combine elemental mapping, (e) Fe, (f) Nb, (g) Mo, (h) Cr, (i) V.

the M23C6 particles along PAGBs. After the nucleation, it acquires the phase also consume the M23C6 precipitates by nucleating and swal-
bulky shape as a result of fast growth rate (Fig. 16(d)). The elemental lowing to it. The combined effect of precipitation hardening and solid
mapping clearly shows the segregation of Mo to internal interfaces. The solution hardening concludes that the creep rupture strength might be
growth of Laves phase also results in swallowing of the M23C6 and other enhanced at the initial stage as result of fine Laves phase formation and
useful particles that results in the reduction of creep rupture strength. after that, it drops due to the higher growth rate of the Laves phase.
The evolution of Laves phase results in loss of solid solution hard-
ening due to Mo consumption from solution matrix. The precipitation
3.5. Microhardness before and after creep exposure
hardening effect of Laves phase depends on both the volume fraction of
the precipitates and mean size of the Laves phase. At the initial stage of
The variation in microhardness for as-welded, PWHT and PWNT
the precipitation, fine Laves phase provides effective pinning to sub-
condition before the creep exposure are depicted in Fig. 17(a–c). A
grain boundaries but at the second stage due to higher coarsening rate
great variation in hardness was observed in the as-welded condition.
precipitation hardening effect began to decline. The formation of Laves
However, the heterogeneity get reduces in PWHT condition. In PWNT

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Fig. 15. a) Microstructure of ICHAZ in PWNT 2 condition used for EDS spectra, line mapping and elemental mapping, (b) line mapping, (c) EDS spectra of particle;
elemental mapping (d) Fe, (e) Nb, (f) Mo, (g) Cr, (h) V.

Fig. 16. Different stages of Laves phase nucleation, (a) as-received microstructure, (b) segregation of Mo particles along the subgrain boundary during creep
exposure, (c) nucleation and rod-like growth of Laves phase in direction of subgrain boundary, (d) bulky shape Laves phase in thelast stage.

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Fig. 17. Microardness variation for crept specimen with sites of Vicker’s hardness measurement (a) For as-welded crept specimen, (b) for PWHT crept specimen, (c)
for crept PWNT specimen.

condition, a negligible hardness variation is observed. After the creep • The PWHT as per recommended at 760 °C for 2 h resulted in a
exposure, in as-welded condition 1, fracture occur in the base zone homogenized hardness distribution along the welds joint. However,
however in as-welded 2 condition fracture occurs in the FGHAZ. For the creep exposure eventually differentiates the heterogeneous re-
low-stress regime, the hardness is measured to be much lower than the gion across the heat affected zones and make it highly susceptible
as-welded material. In as-welded 1 and as-welded 2 conditions, hard- region towards the Type IV failure.
ness near the crack tip are measured 179 HV (base zone) and 182 HV • The creep rupture life was measured to be higher in the low applied
(FGHAZ). The average hardness of the weld fusion zone was measured stress regime of 150 MPa in each condition of the heat treatments.
to be 307 and 293 HV for as-welded 1 and as-welded 2 conditions, re- However, the maximum creep exposure life was measured for the
spectively. As compared to as-welded condition before creep tests, a PWNT condition in low-stress regime of 150 MPa.
drastic decrease in hardness (436 HV) was noticed after the creep tests. • The PWNT resulted in negligible heterogeneity across the HAZs and
In PWHT condition, variation n hardness after the creep fracture is creep exposure resulted in the failure of the welded joint form the
given in Fig. 17(b). In both the cases, fracture occurs in the FGHAZ base zone instead of the FGHAZ (Type IV).
(Type IV). The hardness near the crack tip was measured 192 and • The PWHTs were observed to be a dominant parameter that governs
177 HV for PWHT 1 and PWHT 2 condition. The average hardness of the microstructure evolution and hardness in the sub-zone of The
the weld fusion zone was measured to be 224 and 222 HV for as-welded P91 weldments. The creep susceptible region (FGHAZ/ICHAZ)
1 and as-welded 2 condition, respectively which was much lower than formed as a result of the weld thermal cycle was remained after the
the average hardness of weld fusion zone before the creep test PWHT and cracking occurred in the FGHAZ during the creep ex-
(236 HV). However, a great variation in hardness is observed for the posure. However, the PWNT resulted in the elimination of creep
low-stress regime of 150 MPa (PWNT 2), as shown in Fig. 17(b). The susceptible region and failure was noticed in the base zone during
variation in hardness for PWNT crept sample is shown in Fig. 17(c). For the creep exposure.
PWNT condition, the hardness was reported to be similar in each zone • The creep susceptible region was shifted form the FGHAZ/ICHAZ to
of the weldments. The hardness measured for the PWNT 1 condition the base zone after the PWNT treatments.
was almost similar to PWNT before creep. However, a great reduction • The PWNT resulted in the formation of coarse precipitates before
in hardness was noticed for the PWNT sample exposed at 620 °C for the creep exposure that showed the higher coarsening rate during
150 MPa. The variation in hardness might be due to softening the effect, the creep exposure and led to the formation of unwanted Mo-rich
grain coarsening and precipitate coarsening. For Both the PWNT crept Laves phase in each zone of the crept sample exposed at 620 °C for
sample, the fracture noticed in the base zone as a result of homogeneity 150 MPa (PWNT 2) which are confirmed form the line and ele-
across the weldments. The hardness measured in the HAZ zone were mental mapping.
208 HV and 193 HV, respectively for PWNT 1 and PWNT 2 condition. • The agglomeration of the precipitates was also detected for the weld
However, the average hardness of weld fusion zone was measured to be fusion zone of PWNT 1 crept sample.
similar for both creep condition and it was 203 HV.

Compliance with ethical standards

4. Conclusions
The authors declare that they have no conflict of interest.
From the study, the following conclusions are drawn;

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