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HEAT TREATMENT INFLUENCE ON THE FATIGUE CRACK PROPAGATION IN A

25 Cr 7 Ni SUPERDUPLEX STAINLESS STEEL

Conference Paper · January 2007

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HEAT TREATMENT INFLUENCE ON THE FATIGUE CRACK PROPAGATION
IN A 25 Cr 7 Ni SUPERDUPLEX STAINLESS STEEL

Vittorio Di Cocco – Università di Cassino, Italy

Ester Franzese – Università di Roma “La Sapienza”, Italy
Francesco Iacoviello – Uiversità di Cassino, Italy
Stefano Natali - Università di Roma “La Sapienza”, Italy

ABSTRACT

The aim of this work is the analysis of the fatigue crack propagation resistance in air of a rolled 25
Cr 7 Ni superduplex stainless steels and the investigation of the microstructure influence on fatigue
crack propagation micromechanisms, considering three different stress ratios (R = 0.1, 0.5, 0.75).
Fatigue specimens used in the experimental tests can be gathered in the following classes according
to the previous thermal cycles performed on the DSS plate (all the heat treatments have been done
in air, LT loading direction):
- solution annealed 1050°C for 1 h (as received)
- 475°C for 1000 h
- 800°C for 1, 3 and 10 h (only R = 0.5)
A scanning electron microscope (SEM) fracture surface analysis has been performed to investigate
the fatigue crack propagation micromechanisms in the investigated superduplex stainless steel.
Experimental results allows to evidence a strong secondary phases, carbides and nitrides influence
on fatigue crack propagation resistance of 25 Cr 7 Ni superduplex stainless steel.

KEYWORDS

Superduplex stainless steel; fatigue crack propagation; damaging micromechanisms

INTRODUCTION

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) [1, 2]. Considering that duplex stainless steels are characterized by really interesting
resistance to pitting and intergranular corrosion, a practical way to classify various duplex stainless
steels is to compare 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.

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Duplex stainless steels are characterized by a two phases microstructure with roughly equivalent
ferrite and austenite volume fractions, and rolled steels exhibit a rolling texture. 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.
Depending on their chemical composition, these steels are prone to age hardening and embrittlement
over a wide temperature range [3, 4]. They are characterized by the presence of two critical
temperature ranges [1, 5], figure 1. The higher critical temperature range (between about 600°C and
1050°C) is characterized by the precipitation of carbides (M23C6, M7C3), nitrides (Cr2N, CrN) and
many intermetallic phases (among them, the most dangerous one is the σ phase). The lower critical
range (between about 350°C and 600°C) is characterized by the ferrite spinodal decomposition and
the precipitation of different intermetallic phases (e.g. G phase) in ferrite grains, usually
corresponding to dislocations or α/γ interfaces [4].

Fig. 1: T.T.T (Transformation–Time–Temperature) diagram for three different austenitic-ferritic

stainless steels [6].

In this work, fatigue crack propagation resistance in air of a rolled 25 Cr 7 Ni superduplex stainless
steels was investigated analysing microstructure influence on fatigue crack propagation
micromechanisms. 25 Cr 7 Ni stainless steel fatigue crack propagation resistance was investigated
both considering as received conditions (solution annealed 1050°C for 1 h), and both the noses in
the TTT diagram (475°C and 800°C respectively). A scanning electron microscope (SEM) fracture
surface analysis was performed in order to investigate the fatigue crack propagation
micromechanisms.

1. MATERIAL AND EXPERIMENTAL CONDITIONS

Chemical compositions and tensile properties of the 25 Cr 7 Ni investigated stainless steel are
shown in table 1. Fatigue crack propagation tests were run according to ASTM E647 standard [7],
using 10 mm thick CT (Compact Type) specimens and considering three different stress ratio values
(R = Pmin/Pmax = 0.1; 0.5; 0.75). Tests were performed using a computer controlled Instron 8501

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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 treatmens
were considered:
- solution annealed 1050°C for 1 h (as received)
- 475°C for 1000 h
- 800°C for 1, 3 and 10 h (only R=0.5)
Experimental results related to da/dN-∆K are interpolated considering the Paris law in the stage II of
III [8]:

da/dN = C ∆Km (1)

where C and m are interpolation parameters, which depend on material, structural state mechanical
properties and environmental test conditions [9].

Table 1: 25 Cr 7 Ni austenitic-ferritic superduplex stainless steel chemical composition (wt%) and

tensile properties (PRE = 42); EN 1.4410; α% = γ% = 50

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. RESULTS AND DISCUSSION

Considering that duplex stainless steel fatigue crack propagation tests results are characterized by a
high repeability [10, 11], only one fatigue test will be considered to investigate heat treatment
influence on 25 Cr 7 Ni superduplex stainless steel.
Fatigue crack propagation resistance in air of solubilized 25 Cr 7 Ni superduplex stainless steel is
characterized by a negligible influence of stress ratio R (figures 2-4), whereas 475°C embrittlement
steel (1000 hours) is characterized by a decrease of the fatigue crack propagation resistance that
depends on the R value. Corresponding to lower R value, solubilized and 475°C embrittled steels
show almost the same behaviour, with a negligible crack growth increase for all the applied ∆K
values (figure 2). Higher R values implies a more and more evident decrease of the fatigue crack
propagation resistance. For R = 0.5 (figure 3), it is evident a decrease of the threshold value ∆Kth,
and a negligible increase of crack growth rate in stage II of III (Paris stage). Finally, for R = 0.75
(figure 4) both a decrease of the threshold value ∆Kth and an evident crack growth rate increase in
stage II of III (Paris stage) are observed after 1000 hours at 475°. High temperature embrittlement
implies a decrease of fatigue crack propagation resistance that depends on the heat treatment
duration (figure 5). After 1 hour at 800°C, the decrease of the threshold value ∆Kth is comparable to
the decrease obtained after an embrittlement at 475°C for 1000 hours; stage II is characterized by a
higher slope, and crack growth rate values are more and more higher, up to five times the
corresponding values of the solubilized steel. After 3 hours at 800°C, it is observed both a decrease
of the threshold value ∆Kth, and an increase of crack growth rate, whereas after 10 hours at 800°C
only a further more decrease of the threshold value ∆Kth is obtained.
Considering that Paris relationship parameter “C” corresponds to a theoretical crack propagation
rate obtained for a ∆K value equal to 1 MPa√m, and parameter “m” corresponds to the slope of the
Paris law in the log(da/dN)-log(∆K) diagram, heat treatment influence on stage II of fatigue crack

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propagation is well represented in figure 6 (R = 0.5). Ranging from the solubilized steel to 475°C
and to 800°C embrittled one, an evident slope increase is obtained. Considering the embrittlement at
800°C, the fatigue crack propagation curve evolution with the embrittlement duration is also clearly
shown with the increase of the log C parameter.

-6
10
R = 0.1
Solubilized
475°C-1000h tempered
-7
10
[m/cycle]
da/dN

-8
10

-9
10

-10
10
3 10 1/2 50
∆K [MPa m ]

Fig. 2: 475°C embrittlement influence on 25 Cr 7 Ni stainless steel fatigue crack propagation

resistance (R = 0.1).

-6
10
R = 0.5
Solubilized
475°C-1000h tempered
-7
10
[m/cycle]
da/dN

-8
10

-9
10

-10
10
3 10 50
1/2
∆K [MPa m ]

Fig. 3: 475°C embrittlement influence on 25 Cr 7 Ni stainless steel fatigue crack propagation

resistance (R = 0.5).

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 -6
10
R = 0.75
Solubilized
475°C-1000h tempered

-7
10
[m/cycle]
da/dN

-8
10

-9
10

-10
10
3 10 50
1/2
∆K [MPa m ]

Fig. 4: 475°C embrittlement influence on 25 Cr 7 Ni stainless steel fatigue crack propagation

resistance (R = 0.75).

-6
10
R = 0.5
Solubilized
475°C - 1000h
800°C - 1h
[m/cycle]

-7 800°C - 3h
10
da/dN

800°C - 10 h

-8
10

-9
10

-10
10
3 10 50
1/2
∆K [MPa m ]

Fig. 5: Heat treatment influence on 25 Cr 7 Ni stainless steel fatigue crack propagation resistance (R
= 0.5).

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 -10,8

log C -11,0 Solubilized

-11,2 800°C - 10h

800°C - 3h
475°C - 1000h
-11,4

-11,6
800°C - 1h

-11,8
2,6 2,8 3,0 3,2 3,4 3,6 3,8
m

Fig. 6: Heat treatment influence on “m-C” Paris relationship parameters.

SEM fracture surface analysis allows to identify heat treatment influence on the main fatigue crack
propagation micromechanism. Solubilized 25 Cr 7 Ni superduplex stainless steel is characterized by
the presence of striations and the absence of secondary cracks (both transgranular and intergranular).
The importance of cleavage is really reduced if compared to other duplex stainless steels (e.g. 22 Cr
5 Ni, [12, 13]), also corresponding to high values of the applied ∆K (figure 7).
For all the investigated R values, the influence of 475°C -1000 hours heat treatment on fatigue
crack propagation micromechanism is characterized by an evident cleavage of ferrite grains also
corresponding to low ∆K values (figure 8). The increase of the applied ∆K implies a more fragile
fracture surface morphology, with the presence of really evident secondary cracks, mainly
transgranular (figure 9), but also partially intergranular.

Fig. 7: Solubilized 25 Cr 7 Ni superduplex stainless steel fracture surface (∆K = 25 MPa√m, R =

0.5; crack grows from left to right).

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Considering the embrittlement at 800°C, fracture morphology depends on the heat treatment
duration:
- after 1 hour, cleavage is evident for all the applied ∆K (figure 8 and 9); secondary crack are
also present, but they are mainly intergranular (interfaces α/γ) and their importance increase
with the applied ∆K;
- after 3 hours, secondary cracks are both intergranular (interfaces α/γ) and transgranular
(inside α grains) , and their importance always increase with the applied ∆K (figures 12 and
13);
- after 10 hours, secondary cracks are mainly transgranular (always inside α grains) and
propagates along the main crack direction; they are more and more important with the
increase of the applied ∆K.
Differences in fracture surface morphology are due to the different secondary phases, nitrides and
carbides that precipitate with their peculiar kinetics, and their peculiar precipitation sites,
corresponding to the investigated heat treatment.

Fig. 8: 475°C – 1000h embrittled 25 Cr 7 Ni Fig. 9: 475°C – 1000h embrittled 25 Cr 7 Ni

superduplex stainless steel fracture surface (∆K = superduplex stainless steel fracture surface (∆K =
15 MPa√m, R = 0.1; crack grows from left to 30 MPa√m, R = 0.1; crack grows from left to
right). right).

Fig. 10: 800°C – 1h embrittled 25 Cr 7 Ni Fig. 11: 800°C – 1h embrittled 25 Cr 7 Ni

superduplex stainless steel fracture surface (∆K = superduplex stainless steel fracture surface (∆K =
10 MPa√m, R = 0.5; crack grows from left to 20 MPa√m, R = 0.5; crack grows from left to
right). right).

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Fig. 12: 800°C – 3h embrittled 25 Cr 7 Ni Fig. 13: 800°C – 3h embrittled 25 Cr 7 Ni
superduplex stainless steel fracture surface (∆K = superduplex stainless steel fracture surface (∆K =
8 MPa√m, R = 0.5; crack grows from left to 18 MPa√m, R = 0.5; crack grows from left to
right). right).

Fig. 14: 800°C – 10h embrittled 25 Cr 7 Ni Fig. 15: 800°C – 10h embrittled 25 Cr 7 Ni
superduplex stainless steel fracture surface (∆K = superduplex stainless steel fracture surface (∆K =
6 MPa√m, R = 0.5; crack grows from left to 12 MPa√m, R = 0.5; crack grows from left to
right). right).

3. CONCLUSIONS

The aim of this work was the analysis of the heat treatment influence on fatigue crack propagation
resistance in air of a rolled 25 Cr 7 Ni superduplex stainless steels and the investigation of the
fatigue crack propagation micromechanisms. 25 Cr 7 Ni stainless steel fatigue crack propagation
resistance was investigated both considering as received conditions (solution annealed 1050°C for 1
h), and two different heat treatment temperatures (475°C for 1000 hours and 800°C for 1, 3 and 10
hours). On the basis of the experimental results, it is possible to summarize the following
considerations:
- Solubilized superduplex 25 Cr 7 Ni is characterized by a really interesting fatigue crack
propagation resistance, with crack propagation micromechanism that are mainly
characterized by a ductile morphology (striations).

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 - Investigated superduplex stainless steel after the investigated heat treatment is characterized
by a decrease of the fatigue crack propagation resistance, with a decrease of the ∆Kth values
and an increase of the fatigue crack growth rates that depend on the heat treatment
conditions;
- Fracture surface morphology is strongly affected by heat treatment conditions. Cleavage is
the common morphology for all the investigated heat treatments, whereas secondary cracks
morphology strongly depends on the heat treatment conditions (temperature and/or
duration).

REFERENCES

1) P. LACOMBE, B. BAROUX, G. BERANGER, Les aciers inoxydables. Les èditions de physique,

Les Ulis Cedex A, France. (1990), p.663.
2) A.J. ALDYKIEWICZ, H.S. ISAACS, Corros. Sci. 40, (1996), p.1627.
3) B. JOSEFSSON, J.-O. NILSSON, A. WILSON, Proc. of Duplex stainless steels 91. Ed.
Physique, 1, (1991), p.67.
4) F. IACOVIELLO, F. CASARI, S. GIALANELLA, Corros. Sci. 47,(2005), p.909.
5) J. CHARLES, Proc. of Duplex stainless steels 91. Ed. Physique, 1, (1991), p.3.
6) J. CHARLES, Proc. Duplex 2000 6th World, Venezia, Italy, (2000), p.1.
7) ASTM Standard test Method for Measurements of fatigue crack growth rates (E647-93), Annual
Book of ASTM Standards (1993), 0301, American Society for Testing and Materials.
8) P.C. PARIS The trend of Engineering at the University of Washington, 13, (1961), p.9.
9) A. IOST, Int. J. of Fatigue, 13, (1991), p.25.
10) F.IACOVIELLO Proc. IGF15 Meeting, Bari, Italy (2000), p.322.
11) F. IACOVIELLO, Int. J. of Fatigue, 22, (2000), p.657.
12) F. IACOVIELLO, M. BONIARDI, G.M. LA VECCHIA, Int. J. of Fatigue, 21, (1999), p.957.
13) M. SOZAŃSKA, F.IACOVIELLO, J.CWAJNA, M.JEROME, J.SOJKA, J.GALLAND, Image
Analysis & Stereology, I.A.S. Acta Stereologica, 21, (2002), p.55.
14) M. GUTTMANN, Proc. of Duplex stainless steels 91. Ed. Physique, 1, (1991), p.79.

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