Materials Science & Engineering A 560 (2013) 678684

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Materials Science & Engineering A

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Long term creep behaviour of welded joints of P91 steel at 650 1C

M.E. Abd El-Azim, O.H. Ibrahim n, O.E. El-Desoky
Metallurgy Department, Atomic Energy Authority, Cairo, Egypt

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

Article history: The martensitic P91 steel (9 Cr1MoVNb) has been used for high temperature components in the
Received 18 July 2012 highly ultra super critical pressure steam power plants. The creep behaviour in terms of creep rupture
Received in revised form strength and minimum creep rate of the welded joints of this steel is controlled by that of the ne-
4 October 2012
grained heat affected zone (FGHAZ). The factors which results in the reduction of the creep rupture
Accepted 5 October 2012
Available online 10 October 2012
strength and the increase in the minimum creep rate of FGHAZ at 650 1C were determined and
discussed. It was found that the main difference between the welded joint zones is the prior austenite
Keywords: grain size. The ner the prior austenite grain size as in FGHAZ, the higher is the rate of recovery of
Martensitic P91 steel dislocations, the rate of coarsening of the subgrain structure and coarsening of the intergranular Cr-rich
Welded joint
carbide particles, consequently, the lower the creep resistance.
Fine grained heat affected zone
& 2012 Elsevier B.V. All rights reserved.
Creep rupture strength

1. Introduction 2. Experimental

Martensitic heat resistant P91 steel (9 Cr1MoVNb) has
been used for the main steam pipes, headers, boilers and other
components in fossil power generation plants because it has the
advantages of low thermal expansion, high thermal conductivity,
good steam corrosion resistance and excellent creep resistance
[1,2]. These advantages allow the steam power plants to operate
at a high steam temperature more than 600 1C and a steam
pressure greater than 300 bar [1].
The martensitic structure of these steels includes considerable
amounts of dislocations in lath structure introduced by quenching
after austenitizing so it has a good creep resistance [1]. However,
in the case of welded joints, the ne grained region of the heat
affected zone (HAZ) has lower creep rupture strength than the
base metal [1,3] and so deteriorates the creep rupture strength of
the welded joints.
The correlation between the creep properties and microstruc-
ture of 9 Cr1MoNbV and 9Cr1MoNbVW steels have been
studied extensively [310]; by contrast there are a few investiga-
tions on the microstructural evolution during creep for their
welded joints [112]. At present, however, the mechanisms
responsible for a drop in the creep strength of these welded
joints are not fully understood [3,13,14]. The aim of this work is to
study the role of microstructural instability of ne-grained HAZ
on the creep behaviour of the welded joint of X10CrMoVNb 91
(P91) steel at 650 1C.
2.1. Material and heat treatment
The material used in this study was P91 steel in the form of a tube
of wall thickness of 85 mm and of outer diameter of 492 mm. Table 1
gives the chemical composition of this steel. This steel was austeni-
tized at 1050 1C for 10 min and air cooled, then tempered at 760 1C
for 2 h and nally air cooled. The welded joints were made by manual
metal arc welding process (MAW) of pipes and given a post weld heat
treatment (PWHT) at 760 1C for 2 h, followed by air cooling. For better
comparison between this steel (base metal) and its welded joint, the
same tempering treatment mentioned above (760 1C for 2 h) followed
by air cooling was applied additionally to this steel.
2.2. Creep test
Creep tests were performed on the base metal and the welded
joints. The tests were carried out at 650 1C, in air and at various
constant applied loads by using single and multi specimens, lever
type creep machines. Cylindrical test specimens with a 36 
12 mm uniform gauge cross section were machined from the base
metal and with a 70  12 mm uniform gauge cross section were
machined from the welded joints. The test specimens of the welded
joints were cross weld specimens where the centre of the weld metal
of the welded joint was the centre of the uniform gauge length.

2.3. Examination techniques

n
Corresponding author. Fax: 02 244620788. The welded joint specimens after PWHT and creep rupture
E-mail address: omyma_essam@yahoo.com (O.H. Ibrahim). tests were subjected to microhardness tests and microstructural

0921-5093/$ - see front matter & 2012 Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.msea.2012.10.013
 M.E. Abd El-Azim et al. / Materials Science & Engineering A 560 (2013) 678684
Table 1
Chemical analysis of P91 steel.
Element (wt.%)
C Si Mn Cr Mo V Nb Ni P S
0.104 0.27 0.46 8.17 0.90 0.194 0.064 0.16 0.014 0.003
investigations. The microstructural investigations were carried
out by means of optical microscopy and transmission electron
microscopy (TEM).
Optical metallographic sections were prepared by mechanical
grinding, polishing down to 1 mm diamond abrasive and etching
in a solution of 100 ml of ethanol, 3 g of picric acid and 1 ml of
HCl. For analytical TEM work thin foil specimens and extraction
replicas were used. The thin foil specimens for TEM were
prepared by mechanical grinding to have nearly 50 mm thickness
and then were double-jet electropolished by using an electrolyte
of 950 ml of CH3COOH(conc.) and 50 ml of HCl(conc.), at 13 1C and
30 V. Extraction replicas were prepared from the metallographic
sections, etched in a solution of 100 ml of HCl(conc.), 10 ml of
HNO3(conc.), 100 ml of H2O and 0.3 ml of Vogels reagent for 1 min,
then immersed one time in a solution of 0.5 g of polyvinylformal
in 100 g of trichloromethane (CHCl3) to have a thin lm from the
surface of the specimen, coated by nitrozellulose and nally
coated by a thin lm (  20 nm) of carbon. The nitrozellulose
was removed from replicas by a solution of isoamylester. The TEM
investigations were performed by a JEM-2000FX (JEOL), operated
at 200 kV, in combination with an energy dispersive of X-ray
spectrometer (EDX, Noran) and with an electron image lter
(EFTEMGaten). The microprobe chemical analyzer was used to
identify the variation in the chemical composition across the
welded joint. The scan area was 5 mm distribution between the
base metal, heat affected zone and weld metal, the total scan area
covered 400 points. The distance between points in HAZ (3 mm)
is 10 mm. This analysis was done for Fe, Cr, Mo and Nb elements.
3. Results
3.1. Microstructure
The microstructure of the different zones of the welded joint of
P91 steel after PWHT, along the axis normal to the fusion line from
the weld metal to the base metal of the welded joint, is shown in
Fig. 1. Fig. 1(a) shows the microstructure of the weld metal zone. It
was found that the HAZ, which started next to the fusion line and
adjacent to the weld metal (WM), Fig. 1, consisted of two regions.
A region of  1 mm width with tempered martensite structure of
coarse prior austenite grains of an average 50 mm size (CGHAZ) was
observed right next to the fusion line (Fig. 1(b)). This was followed
by a region of  2 mm width with also tempered martensite
structure but of ner prior austenite grains of an average 10 mm
size (FGHAZ) (Fig. 1(c)). In the HAZ region, the prior austenite grain
size decreases gradually with increasing distance from the fusion
line. In the base metal region (BM), Fig. 1(d), a tempered martensite
structure exists with prior austenite grains of  30 mm size.
3.2. Microhardness
The microhardness proles for the welded joint after PWHT
and after the long term exposure (14,379 h) at 650 1C and 40 MPa,
along an axis normal to the fusion line (FL) from the weld metal to
the base metal of the welded joint are presented in Fig. 2. The
microhardness was measured by using an indentation load of 1 N
679
(HV 0.1); the fusion line was taken to be zero for the distance
measurement. The microhardness proles reveal 4 distinct
regions. Using the results of the microstructural study in Section
3.1, these regions can be identied as follows:
N
(i) Weld metal region in advance of the fusion line (FL).
0.055 The average values of hardness in this region are 240 HV in
the PWHT condition and 210 HV after creep exposure.
(ii) Coarse-grained HAZ region of nearly 1 mm width right next
to the fusion line. The hardness in this region reaches its
maximum value. The maximum values of hardness are 250
HV in the PWHT condition and 225 HV after creep exposure.
(iii) Fine-grained HAZ region of width of  2 mm. The hardness in
this region decreases with increasing distance from the
fusion line, reaches its minimum value of 200 HV in the
PWHT condition and of 110 HV after creep exposure at a
distance of 2 mm from the fusion line, then increases with
increasing the distance from the fusion line.
(iv) Base metal region of hardness of an average value of 225 HV
after PWHT and 190 HV after creep exposure.
3.3. Microprobe analysis
Fig. 3 shows the chemical analysis across the welded joints of
P91 steel after PWHT and after creep tests at 600 1C/70 MPa
(26,035 h) [15] and at 650 1C/40 MPa (14,379 h) for Fe, Cr, Mo and
Nb elements. The PWHT specimens and the creep specimens
tested at 650 1C for 40 MPa exhibit normal elemental concentra-
tions identical to that of the alloy composition across the welded
joint while the creep specimens tested at 600 1C for 70 MPa
(26,035 h) shows a large scatter in Mo concentration, across the
welded joint.
3.4. Creep behaviour
Fig. 4 shows experimental creep rupture strength vs. log
rupture time plot at 650 1C for the welded joints (WJ) of P91
steel in comparison with the experimental values of the creep
rupture strength of the base metal (BM) of P91 steel. It was found
that, in general, the creep rupture strength of the welded joints is
lower than the creep rupture strength of the base metal.
The creep rupture strength of the welded joints at 650 1C
approaches the creep rupture strength of the base metal after
short term creep tests, while it was much lower than the creep
rupture strength of the base metal after longer term creep tests
(rupture time Z6000 h and stress o70 MPa).
Fig. 5 shows creep curves in terms of strain versus time (et)
for the base metal and the welded joints of P91 steel for uniaxial
tensile creep tests conducted at 65 1C under comparable levels of
the applied stress. At low stresses the creep curves of the base
metal (55 MPa) and the welded joints (40 MPa) show three
stages: primary or transition creep, secondary or steady state
creep followed by tertiary creep. At higher stresses the creep
curves shows primary creep followed by tertiary creep. The
welded joint shows shorter time to fracture than the base metal
at the same applied stress of 55 MPa, where the tertiary creep
starts after nearly 1000 h exposure for the welded joint while it
starts after nearly 20,000 h exposure for the base metal. The et
curves can be replotted in the form of instantaneously strain rate
(creep rate) versus time as shown in Fig. 6. At applied stress of
55 MPa, the base metal of P91 steel shows well dened steady
state creep with a minimum creep rate of 5  10  10 s  1, while the
welded joint shows only primary creep followed by tertiary creep
with a minimum creep rate of 1  10  10 s  1. At 40 MPa the
680 M.E. Abd El-Azim et al. / Materials Science & Engineering A 560 (2013) 678684

W CHA

FHA B

Fig. 1. Microstructures of the different zones of the welded joint of P91 after PWHT: (a) weld metal (b) coarse-grained HAZ (c) ne-grained HAZ (d) base metal.

300 lower than that of the base metal as shown in Fig. 4 and the
After PWHT minimum creep rate at 650 1C and 55 MPa is higher in the welded
After Creep at 650 C and 40 MPa joint than in the base metals and at the same creep condition
(650 1C, 40 MPa) the tertiary creep starts earlier in the welded
250
joint than in the base metal as shown in Fig. 5. The creep
resistance of the welded joints is controlled by the creep resis-
Hardness, HV

tance of their FGHAZ, where the FGHAZ has the lowest hardness
200 in comparison with the other regions of the welded joint after
PWHT and after creep at 650 1C as shown in Fig. 2. In our previous
work [3] we found that the specimens simulated to the FGHAZ
have lower creep resistance than the welded joints at 600 1C.
150 The low creep resistance of the FGHAZ of the welded joints of
P91 steel is due to the following:

1. Softening during creep which results from mainly the growth

100
-2 0 2 4 6
Distance from the fusion line, mm
Fig. 2. Microhardness proles across the welded joints of P91.
welded joint shows nearly well dened steady state creep with a
minimum creep rate of 1  10  10 s  1.
4. Discussion
The welded joints of P91 steel have lower creep resistance
than the base metal of P91 steel after long-term creep test at
650 1C where the creep rupture strength of the welded joints is
of subgrains and the recovery of dislocations within these
subgrains. These subgrains result from the recovery of the
8 10 martensite lath during PWHT by the annihilation of disloca-
tions within the lathes and the removal of low angle lath
interfaces. It was found that the subgrain size of the FGHAZ
increases from 0.718 mm after PWHT to 1.23 mm after creep at
650 1C/40 MPa and the dislocation density decreases from
6.3  109 cm  2 after PWHT to 2.4  109 cm  2 after creep at
650 1C/40 MPa as shown in Table 2 and Fig. 7. It is important to
mention that the FGHAZ is softer than the base metal of the
welded joint where the subgrain size is coarser and the
dislocation density is lower in FGHAZ after PWHT and after
creep in comparison with the base metal of the welded joint as
shown in Table 2 and Fig. 7, after PHWT and during creep.
2. Disappearance of ne M23C6 carbide particles, which hinder
the growth of subgrains by pinning their boundaries. This
results in an increase in the rate of growth of the subgrains,
 M.E. Abd El-Azim et al. / Materials Science & Engineering A 560 (2013) 678684 681

Welded Joint Base Metal

110
100

Rupture Strength, MPa

90
80
70
60
50
40
30
20
100 1000 10000 100000
Rupture Time, h

Fig. 4. Creep rupture strength versus log rupture time plots of P91steel at 650 1C.

0.40
s = 70MPa
0.35
s = 55MPa

0.30

0.25
Strain

0.20

0.15

0.10

0.05

0.00
0 5000 10000 15000 20000 25000
Time, h

0.040
s = 70 MPa
0.035
s = 55 MPa
0.030 s = 40 MPa

Fig. 3. Chemical analysis proles across the weld joints of P91steel: (a) after 0.025
PWHT, (b) after interupted creep test at 600 1C/70 MPa [16], (c) after creep test at
Strain

650 1C/40 MPa. 0.020

i.e., an increase in the rate of softening similar to that found by
Panait et al. [16]. It was found that the M23C6 particles are
coarse with an average size of 158 nm after PWHT and 173 nm
after creep as shown in Table 3. Fig. 8 shows the formation of
the Cr-rich carbide particles with red color after creep test at
650 1C/40 MPa. The formation of C23C6 in P91 steel after PWHT
is conrmed in our previous work [3] and by its red color as
found by Maile [17] and shown in Fig. 8.
3. Particles of V-rich carbonitride (V(C, N)) are ne, of an average
size of 70 nm with green color as shown in Fig. 8 and Table 3
after creep but they precipitate adjacent to the coarse particles
of M23C6 as shown in Fig. 8. This prevents their contribution
to particle strengthening.
4. The disappearance of the Nb-rich carbonitride particles during
creep which were observed as ne particles after PWHT as
shown in Table 3 and the formation of coarse particles of Z
phase (Cr (V, Nb) N) with yellow color and an average size of
0.015
0.010
0.005
0.000
0 2000 4000 6000 8000 10000 12000 14000 16000
Time, h
Fig. 5. Creep curves of P91 steel at 650 1C: (a) base metal, (b) welded joint.
279 nm as shown in Fig. 8 and Table 3 at the expense of
Nb-rich carbonitride particles. The formation of Z phase in P91
steel after long-term creep test at 650 1C and 40 MPa was
conrmed by its chemical analysis by EDX as shown in Table 4
and its yellow color as observed by Maile [17] and shown in
Fig. 8. The formation of Z phase at the expense of the ne
682 M.E. Abd El-Azim et al. / Materials Science & Engineering A 560 (2013) 678684

10-6 In our previous work [3] Lavas phase of coarse particles of

s = 70 MPa 375 nm was observed on the prior austenite grain boundaries and
the subgrain boundaries after long term creep exposure (26,035 h)
s = 55 MPa
at 600 1C/70 MPa in the FGHAZ of the welded joint of P91 steel.
10-7 Although Lavas phase contribution to particle strengthening and its
pinning of subgrain boundaries terminate during creep afterwards
Strain rate (s-1)

due to its high rate of growth at 600 1C, the formation and
coarsening of Lavas phase consumes much more Mo element from
10-8 the matrix and hence decreases the contribution of Mo to the solid
solution strengthening resulting in a reduction of the creep rupture
strength of the matrix. It was found that Mo addition improves the
creep properties of 9% Cr steels through solid solution strengthening
10-9 [21,22].
However, much fewer numbers of particles of Lavas phase
were formed after long-term creep exposure for 14,379 h at
650 1C/40 MPa, where there is very slight variation of Mo con-
10-10 centration across the welded joint in comparison with the long
0 5000 10000 15000 20000
Time (h) term exposure to creep for 26,035 h at 600 1C/70 MPa as shown in
Fig. 3. Very few particles of Lavas phase were observed on the
1E-6 prior austenite grain boundaries and subgrain boundaries after
s= 70 MPa long term creep test (14,379 h) at 650 1C and 40 MPa, the average
s = 55 MPa size of these particles was 775 nm. Thus, the role of formation of
Lavas phase during creep at 650 1C can be neglected.
s = 40 MPa
1E-7 The last four factors of softening mentioned above generally
play the same role, but with lower rate in reducing the creep
Strain rate (s-1)

resistance of the coarse-grained HAZ, the base metal and the weld
metal of the welded joint of P91 steel in comparison with the ne
1E-8 grained HAZ. It was found that the main difference between these
regions of the welded joint is the prior austenite grain size. The
prior austenite grains enhance the recovery of martensite sub-
grains as found by Kimura et al. [8]. Thus, the higher the grain
1E-9
boundary area per unit volume as in the ne grained HAZ in
comparison with the other regions of the welded joint, the higher
is the rate of softening and so the lower is the creep resistance.
1E-10 The contribution of the various microstructural features (disloca-
0 5000 10000 15000 tion density, subgrain size, carbide, nitride and carbonitride particles
and intermetallic (Z and Lavas phases) precipitates to the creep
Time (h)
strength of P91 steel as mentioned above is similar to that reported
Fig. 6. Creep rate versus time plots of P91 steel at 650 1C and different applied in P92 steel by Ennis [7]. During creep a rapid reduction in dislocation
stresses: (a) base metal, (b) welded joint. density associated with an increase in subgrain size occurred. The
increases of M23C6 precipitate size which eliminates its effect on the
Table 2 growth of subgrains, the precipitation of coarse intermetallic Lavas
The Average subgrain size and dislocation density for P91 welded joint before and precipitates and Z phase which consume the effective elements (Mo
after creep at 650 1C/40 MPa. and Nb) that contribute in increasing the creep strength and the
formation of the ne particles of V-rich carbides adjacent to the
Condition Dislocation Subgrain
density (cm  2) size (lm) coarse Cr-rich carbides inhibits their role in particle strengthening
indicates that the creep behaviour of martensitic P91 steel of
BM of welded joint after PWHT 15.7  109 0.458 polygonal subgrains is mainly controlled by the dislocation substruc-
BM of welded joint after creep 8.7  109 0.597
ture where dislocation substructure dominates the role of precipita-
FGHAZ after PWHT 6.3  109 0.718
FGHAZ after creep 2.4  109 1.230 tions strengthening due to nitride and carbide particles.
It should be noted that tertiary creep has started earlier in the
welded joint than in the base metal at the same applied stress.
This is due to the higher rate of softening of the FGHAZ of the
V-rich nitride and Nb-carbonitride was observed in 912 Cr steels welded joint (higher rate of recovery of dislocations and higher
[3,1822] where these particles act as nucleation sites for the Z- rate of coarsening of subgrain boundaries) associated with higher
phase. The ne Nb-rich carbonitride and V-rich nitride particles rate of formation of creep voids as observed in our previous work
serve as effective obstacles to dislocation motion within the [23] in comparison with the base metal.
subgrains as well as the growth of subgrains by pinning their
boundaries resulting in high creep strength [19]. It was found that
the ne particles of V-rich nitride and Nb- carbonitride are
effective obstacles against dislocation glide within the subgrains 5. Conclusions
resulting in a high creep strength in high nitrogen (0.055 wt%) 10
XCrMoNbV steel [12]. Also P91 steel used in this work has the It is concluded that:
same nitrogen content and so the FGHAZ of its welded joint has a
low creep resistance because of the disappearance of the ne Nb- 1. The ne-grained heat affected zone (FGHAZ) of the welded
rich carbonitride particles. joints of P91 steel shows the lowest values of hardness after
 M.E. Abd El-Azim et al. / Materials Science & Engineering A 560 (2013) 678684 683

Fig. 7. (ad): TEM thin foil micrographs of P91 steel welded joints, (a) BM of the welded joint after PWHT, (b) BM of the welded joint after creep at 40 MPa/650 1C,
(c) FGHAZ after PWHT, (d) FGHAZ after creep at 650 1C/40 MPa.

Table 3
Particle size (D) and area fraction of different phases observed in the bright eld micrographs of FGHAZ after PWHT and after creep test at 650/40 MPa.

Condition Cr-rich particle V-rich particle Nb-rich particle Laves phase Z-phase

D (nm) Area (%) D (nm) Area (%) D (nm) Area (%) D (nm) Area (%) D (nm) Area (%)

Post weld heat treatment 158 10.56 57 1.48 61 0.14

After creep 650C/40 MPa 173 16.23 70 1.56 775 Very few 279 7.33

Table 4
Chemical analysis by EDX of Z phase particles observed in the FGHAZ of P91 steel
after creep test at 650 1C/40 MPa.

V Cr Fe Nb Mo

29.8 33.9 7.8 27.2 1.3

PWHT and after creep at 650 1C/40 MPa in comparison with

the other zones of the welded joint.
2. The welded joint of P91 steel has lower creep rupture strength
than the P91 base metal at 650 1C.
3. The P91 steel welded joint shows higher creep rate and its
tertiary creep starts earlier than the base metal at the same
applied stress at 650 1C.
4. The creep behaviour of the welded joint of the P91 steel is
limited by the creep behaviour of its FGHAZ.
5. The main factor which affects the creep resistance of the welded
joint of P91 steel is the prior austenite grain size of martensite.
The ner the prior austenite grain size, as in FGHAZ, the higher is
the rate of recovery of dislocations, the higher are the rates of
coarsening of the subgrain structure and coarsening of the
Fig. 8. CEFTEM Micrograph of an area selected from the ne grained HAZ of the intergranular M23C6 carbide particles, i.e., the higher is rate of
welded joint of P91 steel after creep test at 650 1C and 40 MPa. softening and the lower is the creep resistance.
684 M.E. Abd El-Azim et al. / Materials Science & Engineering A 560 (2013) 678684
Acknowledgment
The authors would like to appreciate the support of Prof.
E. Roos, Dr. H. Rouff and Dr. F. Koufmann, Materialprufungstalt
(MPA), Stuttgart University-Germany for facilitating this work to
be done at MPA through the authors fellowships to MPA.
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