Microstructural Analysis of Simulated Heat Affected Zone

in Creep Resisting Steel

Ljubica Milović1,a, Tomaž Vuherer2,b, Milorad Zrilić1,c, Dejan Momčilović3,d, Slaviša Putić1,e
1
Faculty of Technology and Metallurgy, Karnegijeva 4, Beograd, Serbia
2
Faculty of Mechanical Engineering, Smetanova 17, Maribor, Slovenia
3
Institute for Testing of Materials, Bulevar vojvode Mišića 43, Serbia
a
acibulj@tmf.bg.ac.yu, b tomaz.vuherer@uni-mb.si, c misa@tmf.bg.ac.yu,
d
dejanmomcilovic@yahoo.com, e slavisa@tmf.bg.ac.yu

Keywords: P91, microstructure, simulation of the HAZ, HAZ toughness

Abstract. In the last few decades, the steels intended for use in fossil-fired power plants have been
further developed worldwide. These materials are required to endure the ultra supercritical steam
conditions, increasing their efficiency of power generation. This paper presents the evaluation of
relation between the composition and microstructure of ferritic power plant steel. Microstructure
zones where type IV failures may occur have been studied in details.

Introduction
In the seventies of the past century steel T91 for tubes and steel P91 for thick walled components
(headers and steam lines) were developed. The microstructure of both steels consists of tempered
martensite stabilised by M23C6 carbides with further strengthening due to the presence of
molybdenum in solid solution and a fine distribution of vanadium/niobium rich carbonitride (MX)
precipitates [1]. Experience of using these steels in European power industry (Germany, Denmark)
shows that the steam parameters used approached 300 bar and 600°C, representing net efficiencies
in the range of 45-46% for an inland location [2].
This paper presents the evaluation of relation between the composition and microstructure of
ferritic power plant steel.

Experimental
Material. For this investigation, a tube of P91 steel with 320 mm diameter, wall thickness t = 14
mm and 140 mm long was used. Chemical composition of steel P91 tested in this work is given in
Table 1.

Table 1. Chemical composition of tested material, mas.%

C Si Mn P S Cr Ni Cu Al Mo As
0.120 0.289 0.396 0.009 0.002 8.04 0.080 0.082 0.024 0.850 0.007
W Sb Co N Ti B V Nb
0.013 0.0091 0.012 0.0400 0.003 0.0002 0.242 0.073

The structure of parent metal consisted of tempered lath martensite. On some boundaries of prior
austenitic grains, the presence of isolated coarser carbides exceeding 1µm was observed, Fig. 1.
 Fig. 1. Microstrucure of base P91 steel

Typical temperatures of transformation during the welding cycle were determined from
dilatometric curve, and these are Ac1=835°C and Ac3=930°C. Heating rate was 53.8 °C/s. During
cooling, formation of martensite started at temperature of 375°C, while martensite transformation
completed at temperature of 210°C, Fig. 2. Martensite formation was preceded by separation of a
smaller quantity of bainite.

Fig. 2. Dilatometric curve of P91 steel tested in this work

Simulation. Evaluation of the effects of various welding thermal cycles on microstructure and
mechanical properties of test material using thermal simulator SMITWELD, the specimens
11x11x70 mm were used. Different heat affected zone (HAZ) microstructures were obtained by
simulation of single-pass welding at temperatures of 1386°C, 1300°C, 1250°C up to 950°C, graded
by 50°C, 925°C, 900°C and 850°C and with cooling time between 800°C and 500°C, t8/5, 40 sec.
After welding, the samples were subjected to post-weld heat treatment (PWHT) at 730°C for 1
hour, Fig.3.
All samples were subjected to inspection of microstructure and measurement of hardness. For
examination on scanning electron microscope (SEM), the samples heated to maximum temperatures
of 1300°C and 925°C were chosen and subjected to PWHT.
 Fig. 3. Schematic presentation of thermal cycle of welding and subsequent heat treatment

Results and Discussion

Grain size was homogeneous up to temperature of 1000°C. There was no abnormal grain growth, as
the grain growth most probably was governed by vanadium-nitride (VN) and niobium-nitride
(NbN) precipitates [3]. Starting from 1150°C, different grain size caused by incomplete
recrystallisation was observed, with the following minimum and maximum grain size, Table 2.

Table 2. Grain size determined in accordance to Table 3. Statistic data on measured equivalent
ASTM E 112-96 [4] diameters fr MX carbides
Simulated zone Minimum Maximum 925°C 1300°C
grain size grain size Mean 0.289731665 0.167564
of temperature
Standard Error 0.00908727 0.004205
Tp[°C] Standard 0.222406165 0.063359
1150 10.5 8.5 Deviation
Sample 0.049464502 0.004014
1200 10 7
Variance
1300 9.5 6.5 Minimum 0.112837785 0.112838
1386 9 5.5 Maximum 2.477296965 0.541151
Count 599 227

The appearance of microstructures at temperatures of 925°C, 1100°C, 1300°C and 1386°C is

shown in Fig. 4.
The microstructure corresponding to austenitisation temperature of 925°C, Fig. 4a), consists of
martensite with less prominent martensite laths. Dilatometric curve, Fig. 2, shows that in addition to
martensite, up to simulation temperature of 1150° and with cooling time t8/5 of 40 sec, certain
quantity of bainite formed due to incomplete solubility of carbide phase and reduced content of
alloying elements in solid solution of austenite, which caused the decrease of tempering-hardening
capacity. Based on dilatometric curve, Fig. 2, percentage of transformation of ferrite into austenite
was determined to be approx. 90%. At some prior austenitic grain boundaries, the presence of
coarser carbides above 1 µm was observed. The presence of the carbides is most probably the result
of short time spent on austenitisation temperature, considering that the carbides of M23C6 type
completely dissolve at temperatures above 900°C [3].
a) Tp= 925°C b) Tp= 1100°C

c) Tp= 1300°C d) Tp= 1386°C

Fig. 4. Microstructure of simulated samples – opticam microscopy (temperature and
magnification are designated at each microphotograph)

The microstructure corresponding to austenitisation temperature of 1100°C, Fig. 4b), consists of

tempered martensite with clearly visible martensite laths. Coarser carbide particles above 1µm are
still present.
The microstructure corresponding to austenitisation temperature of 1300°C, Fig. 4c) and 1386°C,
Fig. 4d, also represents tempered lath martensite. Carbide particles above 1µm at the prior austenite
grain boundaries practically are not present.
The application of SEM enables more detailed analysis of distribution and size of the carbides of
M23C6 type, most frequently separated at the boundaries of previously austenitic grains and at the
boundaries of martensite laths as well. In Fig. 5a), one can see that M23C6-type carbides are coarser
at the boundaries of previously austenitic grains than those separated at the boundary of ferritic
subgrains. Distribution of carbide phase M23C6 after digital image post processing of Fig. 5a) is
shown in Fig. 5b), and the results of measurement of carbide surface distribution in Fig. 5c).
Resulting photos and diagram for Tp= 1300°C are shown in Figs 5d), e) and f). By comparison of
photos in Figs 5a) and b) with 5d) and e), one can see that quantity and size of the carbides present
in the sample treated at 1300°C are significantly smaller, which is also confirmed by the results of
statistic distribution of equivalent carbide diameter shown in Fig. 5c) and 5f) and given in Table 3.
Beside the carbides of M23C6-type, a significant role is that of carbonitride precipitates MX tested
by transmission electron microscopy [5]. In present paper, this type of carbonitrides has not been
tested.
a) Tp= 925°C d) Tp= 1300°C

b) Tp= 925°C- carbide distribution e) Tp= 1300°C- carbide distribution

300 120.00% 80 120.00%
70
250 100.00% 100.00%
60
80.00%
Frequency

200 80.00% 50
Frequency

40 Frequency 60.00%
150 60.00%
Frequency 30 Cumulative %
40.00%
100 Cumulative % 40.00% 20
20.00%
10
50 20.00%
0 .00%
0 .00%
19 46 9
22 0 4
11 5 9
2 3 4
28 0 5
3 6 8
42 71 3
34 2
31 M 46

39 2 8
45 7 7
4 8 2
51 42 1
96 6
1
36 17 re
0. 99 199
0. 85 21
0. 70 042
0. 28 464
0. 556 778
0. 41 885
0. 412 307
69 50

0. 98 28
0. 83 571
0. 54 993
0. 840 836
25 57
79
0. 7 o
1
7
54 82
47

80 5
1
47 64
03

91 75
05

17 17

87 68

16 9
91

78

4
49 91

83

0. 413
1
11 34

1. 908

5
29 13

3
1. 439

2
37 95

2
0. 356

0. 395

0. 837

2
1. 210

1. 067

2. 618

77
3

1
09

0.

0.
11

5
09

88
40

60

90

98

68

18
2

1.

eqivalent diametar [µm]

0.

0.

1.

2.

eqivalent diametar [µm]

c) Tp= 925°C- distribution of equivalent f) Tp= 1300°C- distribution of equivalent

diameter of carbide phase diameter of carbide phase
Fig. 5. Microstructure of simulated samples - SEM

Hardness. Hardness of parent metal of 230 HV1 was measured. Variation of hardness of simulated
samples with temperature of simulation showed a drop at 925°C, Fig. 6, and that is why this
temperature of 925°C was chosen as typical for examination. A significant drop of hardness of
almost 40HV occurs at simulation temperature of 850°C that is somewhat above AC1 temperature.
With an increase of simulation temperature, ferrite fraction transforming into austenite increases. At
temperature of 925°C, this fraction was approx. 90%. At this temperature, there was no
considerable dissolution of carbides and nitrides and transformation of C and N into solid austenite
solution. Therefore, martensite formed at cooling had significantly lower content of C and N. Due
to decreased content of C and N, repeated separation of M23C6 carbides and MX carbonitrides
during subsequent heat treatment was limited resulting in hardness lower than that of base metal.
Besides, carbonitride precipitates MX coarsed-became rough and coagulated, which reduced their
hardening effect. Due to the phenomena specified, FGHAZ corresponding to simulation-
temperature interval from 900 to 950°C had the smallest hardness. With an increase of simulation
temperature above 950°C, hardness increased due to higher solubility of carbides.
500

450

400

350

300
Hardness HV

250

200 Specimens with PWHT HV10"

Specimens without PWHT HV5"
150 Base metal HV1"

100

50

0
850 900 925 950 1000 1050 1100 1150 1200 1250 1300
Tp [°C]

Fig. 6. Measured hardness of tested samples

Conclusion
It is necessary to investigate in more details the effect of the technology of manufacture of the
components made of steel P91, including final heat treatment (normalisation + tempering), on the
state of carbide phase in them, and through it on the structure in FGHAZ. Optical microscopy does
not enable complete determination of the structure properties that are essential for fitness for
purpose of the components and weld joints made of steel P91, about which care should be taken
when defining the requirements according to item S6 of the ASTM 335-03 standard.

Acknowledgement
The authors express their appreciation to Ivo Blačić from the Belgrade Military Technical Institute,
for invaluable help and suggestions in writing this paper.

References
[1] J. A. Francis, W. Mazur and H.K.D.H. Bhadeshia: Type IV cracking in ferritic power plant
steels, Materials Science and Technology Vol. 22, No12 (2006), p.1387-1395
[2] Materials & Components in Fossil Energy Applications, A newsletter of the U. S. Department
of Energy’s Office of Fossil Energy Advanced Research Materials Program, Number 162,
(2005)
[3] L. Cipolla, A. Di Gianfrancesco and O. Tassa: Production Experience of TenarisDalmine
T/P91: Microstructure and Mechanical Properties, Creep Behaviour and Microstructural
Evolution, Industry and research Experience in the Use of P91/T91 in HRSG and
Conventional Boilers, London, (2005), p.1040-1110
[4] Standard test Methods for Determining Average Grain Size, ASTM E 112-96, (1996)
[5] P. Mayr and H. Cerjak: Study of the Simulated HAZ of a Boron Alloyed Creep Resistant 9%
Chromium Steel
[6] Standard Specification for Seamless Ferritic Alloy-Steel Pipe for High-Temperature Service,
ASTM A 335/a 335M-03, (2003)