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XXIV Italian Group of Fracture Conference, 1-3 March 2017, Urbino, Italy
XXIV Italian Group of Fracture Conference, 1-3 March 2017, Urbino, Italy
High temperature embrittled duplex stainless steels: influence of the
High temperature
XV Portuguese
chemicalConference embrittled
on Fracture,duplex
composition PCF 2016,
on stainless
the fatigue 10-12 February steels:
crack 2016,influence of Portugal
Paço de Arcos,
propagation the
chemical composition on the fatigue crack propagation
Thermo-mechanical
Francesco Iacovielloa,*, modeling
Vittorio Di of Cocco a high
a
, Ester pressure
Franzesea,turbine bladeb of an
Stefano Natali
Univestià di Cassinoairplane gas turbine
Francesco Iacoviello *, a,
Vittorio Di Cocco a
, Esterengine
Franzese , Stefano Natalib
a
a
e del Lazio Meridionale, via G. Di Biasio 43, 03043 Cassino (FR), Italy
Univestià Università
di Cassino di Roma “Sapienza”, DICMA,
via G.via
Di Eudissiana 18, Roma, Italy(FR), Italy
b
a
e del Lazio Meridionale, Biasio 43, 03043 Cassino
a b c
b
P. Brandão , V. Infante , A.M. Deus *
Università di Roma “Sapienza”, DICMA, via Eudissiana 18, Roma, Italy

a
Department of Mechanical Engineering, Instituto Superior Técnico, Universidade de Lisboa, Av. Rovisco Pais, 1, 1049-001 Lisboa,
Abstract Portugal
b
Abstract IDMEC, Department of Mechanical Engineering, Instituto Superior Técnico, Universidade de Lisboa, Av. Rovisco Pais, 1, 1049-001 Lisboa,
Austenitic-ferritic (duplex) stainless steels are successfully used Portugal
in chemical, nuclear, oil and gas industries, due to their good
c
CeFEMA, Department of Mechanical Engineering, Instituto Superior Técnico, Universidade de Lisboa, Av. Rovisco Pais, 1, 1049-001 Lisboa,
mechanical properties
Austenitic-ferritic and excellent
(duplex) stainlessgeneralized and localizedused
steels are successfully corrosion resistance
in chemical,
Portugal
in many
nuclear, oilenvironments and operating
and gas industries, conditions
due to their good
(for example,
mechanical chloride and
properties induced stressgeneralized
excellent corrosion).and localized corrosion resistance in many environments and operating conditions
The aim of this
(for example, work induced
chloride is the analysis of the influence of the chemical composition and of the high temperature embrittlement
stress corrosion).
processes
The in this
aim of
Abstract threework
different
is theduplex
analysisstainless
of thesteels. Scanning
influence of theelectron
chemicalmicroscope
composition(SEM)
and fracture surface
of the high analysis was
temperature performed
embrittlement
to investigate
processes the fatigue
in three crack
different propagation
duplex stainlessmicromechanisms.
steels. Scanning electron microscope (SEM) fracture surface analysis was performed
© During
to 2017 Thetheir
investigate Authors. Published
theoperation,
fatigue crack by Elsevier
propagation
modern B.V.
aircraftmicromechanisms.
engine components are subjected to increasingly demanding operating conditions,
Copyright
Peer-review © 2017
especially under The Authors. Published
responsibility
the high pressure by
of ElsevierElsevier
the(HPT)
Scientific B.V. This isconditions
Committee an
ofopen
IGF access
causearticle
Ex-Co. theseunder
partsthe
to CC BY-NC-ND license
© 2017 The Authors. Publishedturbine
by blades.
B.V. Such undergo different types of time-dependent
(http://creativecommons.org/licenses/by-nc-nd/4.0/).
degradation,
Peer-review underone of which is
responsibility creep.
of theA model using
Scientific the finite
Committee of element
IGF method
Ex-Co. (FEM) was developed, in order to be able to predict
Peer-review under responsibility of the Scientific Committee of IGF Ex-Co.
the creep
Keywords: behaviour
Duplex StainlessofSteels;
HPTFatigue
blades. Flight
crack data records
propagation; (FDR) forembrittlement.
High temperature a specific aircraft, provided by a commercial aviation
company,
Keywords: wereStainless
Duplex used toSteels;
obtain thermal
Fatigue crackand mechanical
propagation; Highdata for three
temperature different flight cycles. In order to create the 3D model
embrittlement.
needed for the FEM analysis, a HPT blade scrap was scanned, and its chemical composition and material properties were
1. obtained.
IntroductionThe data that was gathered was fed into the FEM model and different simulations were run, first with a simplified 3D
rectangular block shape, in order to better establish the model, and then with the real 3D mesh obtained from the blade scrap. The
1. Introduction
overall expected behaviour in terms of displacement was observed, in particular at the trailing edge of the blade. Therefore such a
Duplex
model canstainless
be usefulsteels
in the (DSSs) are in between
goal of predicting turbinethe austenitic
blade and
life, given theofferritic
a set grades, combining the best mechanical
FDR data.
andDuplex
corrosion resistance
stainless steelsproperties
(DSSs) are ofinboth. As a the
between result of theirand
austenitic highthemechanical strength,
ferritic grades, good thermal
combining the bestconductivity
mechanical
and excellent
© corrosion
2016 corrosion
resistance
The Authors. resistance
properties
Published DDSs
of
by Elsevier are
both. Asextensively
B.V. used high
a result of their both mechanical
in pulp andstrength,
paper industries, in chemical
good thermal and
conductivity
petrochemical
and plants.
excellentunder
Peer-review corrosionThey also of
find
resistance
responsibility some
DDSs
the applications
are
Scientific Committeeinoffood
extensively PCFand
used both
2016.biomedical
in pulp and fields as well,
paper Fruytier
industries, in (1991),
chemicalGunn
and
(1997). The wide
petrochemical useThey
plants. of DSSs is closely
also find connected in
some applications to food
theirand
specific microstructure,
biomedical formed
fields as well, by roughly
Fruytier equal
(1991), Gunn
Keywords:
(1997). TheHigh
percentages Pressure
ofwide use Turbine
austenite ofand
DSSsBlade;
isCreep;
ferrite. Such Finite
closely Element Method;
an connected
austenite-ferrite3D Model;
ratio
to their Simulation.
gives
specific amicrostructure,
higher yield and ultimate
formed by tensile
roughlystrength
equal
percentages of austenite and ferrite. Such an austenite-ferrite ratio gives a higher yield and ultimate tensile strength

* Corresponding author. Tel.: +39.07762993281

* Corresponding iacoviello@unicas.it
E-mail address:author. Tel.: +39.07762993281
E-mail address: iacoviello@unicas.it
2452-3216 © 2017 The Authors. Published by Elsevier B.V.
Peer-review underThe
* Corresponding
2452-3216 © 2017 responsibility
author. of218419991.
Tel.: +351
Authors. theby
Published Scientific Committee of IGF Ex-Co.
Elsevier B.V.
Peer-review under responsibility
E-mail address: of the Scientific Committee of IGF Ex-Co.
amd@tecnico.ulisboa.pt

2452-3216 © 2016 The Authors. Published by Elsevier B.V.

Peer-review under responsibility of the Scientific Committee of PCF 2016.
Copyright © 2017 The Authors. Published by Elsevier B.V. This is an open access article under the CC BY-NC-ND license
(http://creativecommons.org/licenses/by-nc-nd/4.0/).
Peer-review under responsibility of the Scientific Committee of IGF Ex-Co.
10.1016/j.prostr.2017.04.055
 Francesco Iacoviello et al. / Procedia Structural Integrity 3 (2017) 308–315 309
2 Author name / Structural Integrity Procedia 00 (2017) 000–000

than the austenitic grades, with good ductility and toughness. On the other hand, the marked microstructural anisotropy
of these hot rolled materials can result in variability of mechanical properties, such as tensile strength and fracture
toughness, Roberti (1993). The high chromium (between 21 and 27 wt.%) and molybdenum (up to 4.5 wt.%) contents
allow the use of DSSs under conditions of pitting, crevice and, above all, stress corrosion cracking that would be
critical for the traditional AISI 304 and 316. Finally, some economical advantages follow as a result of lower nickel
content than the austenitic grades. The aforementioned mechanical and corrosion resistance properties are achieved in
commercially wrought DSSs after hot rolling followed by a solution annealing and quenching. Hot rolling and solution
annealing parameters (e.g. temperatures, times and strain reductions) for DSS depend on the chemical composition,
the desired ferrite/austenite volume ratio, the final plate thickness, Charles (2008). Partition coefficients for a given
element do not vary with the steel chemical composition: ferrite grains result to be enriched in P, W, Mo, Si and Cr,
whereas austenite grains are enriched in N, Ni, Cu and Mn.
Considering that DSSs are characterized by really interesting resistance to pitting and intergranular corrosion, a
practical classification criterion of various DSS is based on their pitting index, or pitting resistant equivalent (e.g.
PRE= %Cr + 3.3 (%Mo + 0.5%W) + 16 %N ). Among duplex stainless steel, at least three different types can be
identified:
- “lean” duplex, that are characterized by very low Mo and Ni content, with a PRE that is about 25(they can be
considered as valid substitute of AISI 304);
- duplex with a PRE of about 35; 22 Cr 5 Ni duplex stainless steel can be considered as the standard alloy;
- “superduplex” stainless steels having PRE values greater than 40 (they are characterized by a corrosion
resistance that is comparable to superaustenitic steels and can be used in very aggressive environment).
Depending on their chemical composition, these steels are prone to age hardening and embrittlement over a wide
temperature range, Iacoviello (2008). DSSs are characterized by two embrittling temperature ranges (C-shaped curves)
which exhibit several secondary phases, carbides and nitrides precipitation at different holding times. A representative
TTT diagram showing the above mentioned phenomena for SAF 2304, 2205 and 2507 grades is reported in Fig. 1.

Fig. 1: TTT diagram for DSSs: chemical composition influence, Redjajmia (1991).

A first critical temperature range is situated between 500° and 1100°C, and it involves the formation of carbides
(M7C3 and M23C6), nitrides (Cr2N and ), secondary austenite 2, , R, and  phases depending upon the steel
composition and its thermal conditions, Wang (1991)  phase, as a result of the fact it is present in a large volume, is
the most important phase besides ferrite and austenite.
A second critical temperature range is between 350°C and 500°C with a nose at about 475°C. In this temperature
range two mechanisms can be related to the so called “475°C embrittlement” of the steel, Guttman (1991) and
Iacoviello (2005):
- a spinodal decomposition of the a ferrite in two phases: an a9 Cr-rich phase and an a Fe-rich phase.
- nucleation and growing of Ni-Si-Mo rich f.c.c. G phase, characterized by a very slow precipitation kinetic (the
overall concentration in “G-forming” elements increases from 40 to 60% between 1000 and 30000 h at 350°C).
Mechanical properties are strongly influenced by these changes in microstructure, Iacoviello (1997).
310 Francesco Iacoviello et al. / Procedia Structural Integrity 3 (2017) 308–315
Author name / Structural Integrity Procedia 00 (2017) 000–000 3

In this work, three different austenitic stainless steel were considered, ranging from a “lean” chemical composition
to a “super” duplex grade. Fatigue crack propagation resistance was investigated in air considering stress ratio
influence and high temperature tempering treatment (800°C), ranging from 1 to 10 hours. Crack propagation
micromechanisms were investigated by means of a scanning electron microscope (SEM) fracture surface analysis.

2. Investigated steels and experimental procedure

Investigated rolled stainless steels chemical composition and tensile properties are shown in tables 1-3. All the
investigated steels are characterized by analogous ferrite/austenite ratio ( = 1) and show a rolling texture. Fatigue
crack propagation tests were run according to ASTM E647 standard (2015), using 10 mm thick CT (Compact Type)
specimens and considering three different stress ratio values (R = Kmin/Kmax = 0.1; 0.5; 0.75). Tests were performed
using a computer controlled Instron 8501 servohydraulic machine in constant load amplitude conditions (sinusoidal
loading waveform) at room temperature, with a loading frequency of 30 Hz. Crack length measurements were
performed by means of a compliance method using a double cantilever mouth gage. Different heat treatments were
considered:
- solution annealed 1050C for 1 h (as received);
- 800C for 1, 3 and 10 h (only R0.5).
Fatigue crack propagation micromechanisms were investigated by means of SEM fracture surface analysis,
considering loading conditions (R and applied K) influence.

Table 1: 21 Cr 1 Ni “lean” DSS chemical composition (wt%) and tensile properties (PRE = 26); EN 1.4162.
C Mn Cr Ni Mo N
0.03 5.00 21.5 1.5 0.3 0.22
YS [MPa] UTS [MPa] A%
483 700 38

Table 2: 22 Cr 5 Ni DSS chemical composition (wt%) and tensile properties (PRE = 35); EN 1.4462.
C Mn Cr Ni Mo N
0.019 1.51 22.45 5.50 3.12 0.169
YS [MPa] UTS [MPa] A%
565 827 35

Table 3: 25 Cr 7 Ni superduplex stainless steel (SSS) chemical composition (wt%) and tensile properties (PRE = 42); EN 1.4410.
C Mn Cr Ni Mo N
0.019 0.80 24.80 6.80 3.90 0.30
YS [MPa] UTS [MPa] A%
556 814 31

3. Experimental results and discussion

Fig. 2 shows chemical composition influence on DSS fatigue crack propagation in air. Duplex 2205 and
superduplex 2507 stainless steels are characterized by an analogous fatigue crack propagation resistance, for all the
investigated stress ratio values (ranging from 0.1 to 0.75). “Lean” DSS 2101 is characterized by lower threshold values
(for all the investigated R values); furthermore, 2101 DSS is characterized by higher crack growth rate values, for all
the investigated loading conditions (R and K values), up to five times with respect to crack growth rate values
obtained with duplex or superduplex stainless steels. Considering the same loading conditions, SEM fracture surface
analysis confirm that crack propagation micromechanisms are the same in duplex and superduplex stainless steel, with
striation and some secondary cracks for lower K and R values (Fig. 3; crack propagates from left to right) and an
increasing importance of ferrite grain cleavage corresponding to more critical loading conditions (higher K and R
values; Fig. 4). Solution annealed “lean” DSS fracture surfaces are characterized by a more evident importance of
cleavage (Figs. 5 and 6), also considering less critical loading conditions (lower K and R values). Striations are also
observed. Embrittling conditions influence on fatigue crack propagation resistance is shown in Figs. 7-9.
4 Francesco
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000–000 311

-6
10

-7
10

[m/cycle]
da/dN
2101
-8 R = 0.1
10 R = 0.5
R = 0.75
2205
R = 0.1
R = 0.5
-9
10 R = 0.75
2507
R = 0.1
R = 0.5
R = 0.75
-10
10
3 10 1/2
50
K [MPa m ]

Fig. 2: Chemical composition influence on DSSs fatigue crack propagation resistance (solution annealed conditions).

Fig. 3: Solution annealed 2205 DSS fracture surface (K = 15 Figure 4: Solution annealed 2205 DSS fracture surface (K = 25
MPa√m; R = 0.5). MPa√m; R = 0.5).

Heat treatment influence on investigated DSSs is strongly influenced by DSS chemical composition:
- 2101 DSS shows an increase of the threshold value Kth, from about 5 MPa√m (solution annealed) to about 10
MPa√m (800°C-3h); longer tempering duration at 800°C is characterized by a decrease of Kth; final rupture
values decrease with the increase of the tempering duration at 800°C (highest value is obtained with the solution
annealed steel).
- 2205 DSS shows threshold values Kth that practically do not depend on the heat treatment (about 7 MPa√m for
all the investigated heat treatment); the increase of the duration of the 800°C tempering implies a strong increase
of the crack growth rate obtained for the same loading conditions (e.g., for K = 10 MPa√m, differences between
solubilized DSS and the 800°C-10 hours embrittled DSS are higher than a factor of one).
- 2507 DSS is characterized both by a strong decrease of the threshold value Kth and by a strong increase of crack
growth rate values, with the increase of the 800°C tempering duration; the worst fatigue crack propagation
312 Francesco Iacoviello
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behavior is obtained after 10 hours at 800°C (lowest threshold values Kth and highest crack growth rates for the
same K value).

Fig. 5: Solution annealed 2101 “lean” DSS fracture surface (K = 6 Fig. 6: Solution annealed 2101 “lean” DSS fracture surface (K = 11
MPa√m; R = 0.5). MPa√m; R = 0.1).

-6
10

-7
10
[m/cycle]
da/dN

-8
10

-9 2101 (R = 0.5)
10 solution annealed
800°C - 1h
800°C - 3h
800°C - 10h
-10
10
3 10 1/2
50
K [MPa m ]
Fig. 7: 2101 “lean” DSS fatigue crack propagation resistance: heat treatment influence (R = 0.5).

Also crack propagation micromechanisms are influenced by heat treatment conditions. Considering near threshold
conditions, 2101 tempered at 800°C for 1 hour and 3 hours are characterized by fatigue striations, without cleavage
and secondary cracks (Fig. 10). Longest duration of 800°C tempering treatment imply an increase of cleavage
importance with some secondary cracks.
Considering both 2205 and 2507 DSS (Figs. 11 and 12, respectively), ferrite grains cleavage and secondary cracks
are more and more evident with the increase of the 800°C tempering duration.
The different influence of 800°C tempering on fatigue crack propagation resistance is probably due to different
secondary phases, carbides and nitrides precipitation kinetics.
Although 2101 TTT diagram is not available, the analysis of Fig. 1 allows to hypothesize that the really low Ni
content and the high Mn content that characterize 2101 “lean” DSS imply a strong TTT diagram modification, with
different precipitation kinetics if compared to the “standard” 2205 and the “super” 2507 DSS. Fatigue crack
 Francesco Iacoviello et al. / Procedia Structural Integrity 3 (2017) 308–315 313
6 Author name / Structural Integrity Procedia 00 (2017) 000–000

propagation micromechanisms in 800°C tempered 2101 DSS do not correspond to a very embrittled steel: higher
critical temperature range in “lean” DSS should be more deeply investigated.
“Standard” 2205 DSS and “super” 2507 DSS are prone to be embrittled due to tempering treatments at 800°C:
fatigue crack propagation micromechanisms are strongly influenced, with an evident increase of the importance of
ferrite cleavage and secondary cracks propagation in ferrite grains or in ferrite/austenite grain boundaries.

-6
10

-7
[m/cycle]

10
da/dN

-8
10

-9 2205 (R = 0.5)
10 solution annealed
800°C - 1h
800°C - 3h
800°C - 10h
-10
10
3 10 1/2 50
K [MPa m ]

Fig. 8: 2205 “standard” DSS fatigue crack propagation resistance: heat treatment influence (R = 0.5).

-6
10

-7
[m/cycle]

10
da/dN

-8
10

-9 2507 (R = 0.5)
10 solution annealed
800°C - 1h
800°C - 3h
800°C - 10h
-10
10
3 10 1/2 50
K [MPa m ]

Fig. 9: 2507 “super” DSS fatigue crack propagation resistance: heat treatment influence (R = 0.5).

4. Conclusions

Austenitic-ferritic (duplex) stainless steels are successfully used in chemical, nuclear, oil and gas industries, due
to their good mechanical properties and excellent generalized and localized corrosion resistance in many environments
and operating conditions (for example, chloride induced stress corrosion). In this work, three austenitic-ferritic
314 Francesco Iacoviello et al. / Procedia Structural Integrity 3 (2017) 308–315
Author name / Structural Integrity Procedia 00 (2017) 000–000 7

stainless steels were investigated (2101, 2205 and 2507) focusing the influence of chemical composition and high
temperature tempering (800°C, from 1 to 10 hours).
On the basis of the fatigue crack propagation results and of the SEM fracture surface analysis, the following
conclusions can be summarized:
- considering solution annealed conditions, “lean” 2101 DSS is characterized by the worst fatigue crack
propagation behavior for all the investigated loading conditions, with a decrease of the threshold values and higher
crack growth rates;
- considering 800°C tempered steels, both “standard” 2205 and “super” 2507 DSSs are prone to be more and
more embrittled with the increase of the tempering duration: as a consequence, an increase of cleavage and secondary
crack importance on fracture surfaces is obtained with the increase of the tempering time;
- 2101 “lean” DSS seems to be less susceptible to be embrittled by a 800°C tempering heat treatment, if
compared to the 2205 and 2507 DSS; this is probably due to differences in secondary phases, carbides and nitrides
precipitation kinetics.

Fig. 10: 2101 DSS fracture surface analysis (threshold conditions). From left to right: 800°C -1h: 800°C – 3h; 800°C – 10h.

Fig. 11: 2205 DSS fracture surface analysis (K = 12 MPa√m; R = 0.5). From left to right: 800°C -1h: 800°C – 3h; 800°C – 10h.

Fig. 12: 2507 DSS fracture surface analysis (K = 12 MPa√m; R = 0.5). From left to right: 800°C -1h: 800°C – 3h; 800°C – 10h.
8 Francesco
Author nameIacoviello et Integrity
/ Structural al. / Procedia Structural
Procedia Integrity
00 (2017) 3 (2017) 308–315
000–000 315

Acknowledgements

Outokumpu S.p.A. is warmly acknowledged.

References

ASTM E647-15e1, 2015. Standard test method for measurement of fatigue crack growth rates.
Charles, J., 2008. Duplex Stainless Steels - a Review after DSS ‘07 held in Grado, Steel Research International, 79, 455-465.
Fruytier, DJA., 1991. Industrial experiences with duplex stainless steel related to their specific properties. Duplex stainless steel ’91, Beaune,
France, 1, 497-510.
Gunn, R.N., 1997. Duplex Stainless steels. Microstructure, properties and applications. Abington Publishing, Cambridge, England.
Guttmann, M., 1991. Intermediate temperature aging of duplex stainless steels. A review. Duplex stainless steel ’91, Beaune, France, 1, 79-92.
Iacoviello, F., Habashi, M., Cavallini, M., 1997. Hydrogen embrittlement on the duplex stainless steel Z2CND2205 hydrogen charged at 200°C.
Materials Science and Engineering A, A224, 116-124.
Iacoviello, F., Casari, F., Gialanella, S., 2005. Effect of “475°C embrittlement” on duplex stainless steels localised corrosion resistance, Corrosion
Science, 47, 909-922.
Roberti, R., Nicodemi, W., La Vecchia, G.M., Basha, Sh., 1993. J-R curve dependence on specimen geometry and microstructure in two austenitic-
ferritic stainless steels. Int. J. Pres. Ves. & Piping, 55, 343-352.
Redjajmia, A., Metauer, G., Gantois, G., 1991. Decomposition of delta ferrite in a Fe-22Cr-5Ni-3Mo-0.03C duplex stainless steel. A morphological
and structural study. Duplex stainless steel ’91, Beaune, France, 1, 119-126
Wang, X.G., Dumortier, D., Riquier, Y., Structural evolution of zeron 100 duplex stainless steel between 550 nd 1100°C. Duplex stainless steel ’91,
Beaune, France, 1, 127-134.