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Materials Science and Engineering A319 321 (2001) 564 568 www.elsevier.


Fatigue softening of X10CrAl24 ferritic steel

Toma s Kruml a,*, Jaroslav Pola k a,b

iz Institute of Physics of Materials, Academy of Sciences, Z ko6a 22, 616 62 Brno, Czech Republic Laboratoire de Me canique de Lille (URA CNRS 1441), Ecole Centrale de Lille, BP 48, 59651 Villeneu6e dAscq Cedex, France

Abstract Cyclic plastic response of X10CrAl24 ferritic stainless steel in a wide domain of plastic strain amplitude was measured. Cyclic hardeningsoftening curves show important cyclic softening during most of the fatigue life. Cyclic stress-strain curves have different slopes in the domain of low and high strain amplitudes. These two domains in cyclic stress strain curve correspond to two types of internal structure as observed by transmission electron microscopy (TEM). The areas of condensed dislocation structure in the interior and the bands of extrusions and intrusions on the surface indicate the localization of cyclic strain. Fatigue softening was discussed in terms of properties of dislocations in b.c.c. structure and localization of the cyclic plastic strain. 2001 Elsevier Science B.V. All rights reserved.
Keywords: Cyclic plasticity; Ferritic steel; Dislocation structures; Cyclic softening; Strain localization

1. Introduction Cyclic plastic loading results in the modication of the internal structure of the material and simultaneous modication of the stress-strain response. An important feature of the cyclic straining of crystalline materials is the redistribution of the cyclic plastic strain in the crystal and its localization in preferred locations. The intensive changes of the internal structure and accompanying changes of the mechanical properties are usually limited to the initial period of cyclic straining. For majority of the fatigue life the quasi-reversible plastic strain is concentrated in the bands of intensive cyclic strain (often called persistent slip bands PSBs). The redistribution of the cyclic plastic strain leads to the modication of the internal structure in these bands and the specic structure of the PSBs is formed. In most materials, the formation of PSBs results in the stabilization of the cyclic stress strain response. The pronounced relief, consisting usually of extrusions and intrusions is formed at the locations where PSBs emerge on the surface [1]. At the tip of intrusions the primary fatigue cracks are initiated. The relation of the mechanical properties, internal structure and surface relief have been amply investi* Corresponding author.

gated in f.c.c. single and polycrystals [1,2] in which mostly stabilized cyclic stress-strain response was found. The studies in b.c.c. materials are limited. Low alloyed ferritic steel has been studied by Roven and Nes [3], Petersmeier et al. [4] and Pohl et al. [5]. In low amplitude domain cyclic softening was found. The effect of carbon content and temperature on the cyclic behavior of a-iron has been recently studied by Sommer et al. [6]. Ferritic stainless steel single crystals with 26% Cr were studied by Magnin et al. [7,8], those with & esta 13.6% Si by S k et al. [9] and those with 30% Si by Kaneko et al. [10,11]. Cyclic hardening was found for medium and high plastic strain amplitudes. The stress strain behaviour and internal structure changes of polycrystalline stainless ferritic steel have not been systematically studied. The subject of the present work is to study the cyclic stress-strain response and internal dislocation structures in of X10CrAl24 ferritic stainless steel with the aim to nd the explanation for observed cyclic softening.

2. Experiment Ferritic X10CrAl24 stainless steel in the form of a bar of 30 mm in diameter was supplied by Thyssen. Chemical composition was B 0.12 C, 0.7 1.4 Si, B

0921-5093/01/$ - see front matter 2001 Elsevier Science B.V. All rights reserved. PII: S 0 9 2 1 - 5 0 9 3 ( 0 1 ) 0 1 0 0 4 - 8

T. Kruml, J. Pola k / Materials Science and Engineering A319 321 (2001) 564 568


1.0 Mn, B 0.04 P, B 0.03 S, 23 26 Cr, 1.2 1.7 Al, all in at.%. The material was hot rolled in the temperature interval 1100 800C and annealed at 800C. The average grain size was 38 mm and strings of carbides lying parallel to the longitudinal direction were detected on the metallographic sections. Cylindrical specimens with 8 mm diameter and 12 mm length were cycled in computer controlled MTS 880 electrohydraulic testing machine. Symmetric strain cycle with the strain rate 2.5 10 3 s 1 was applied. The plastic strain amplitude derived from the halfwidth of the hysteresis loop was kept constant using the

computer outer loop. For small amplitudes the test was started with a lower strain amplitude and it was automatically adjusted using outer loop in order to achieve the desired plastic strain amplitude. This initial period took 3 30 cycles. For surface relief observations a shallow notch was produced in the middle of the gauge length (cylindrical surface having 60 mm in diameter with the axis perpendicular to the axis of the specimen was ground to 0.4 mm depth). The notch was mechanically and electrolyticaly polished. It was observed in Philips XL 30 FEG scanning electron microscope (SEM). For the observations of internal structures, thin plates of about 1 mm in thickness were cut parallel to the specimen axis by a spark cutter. The plates were subsequently thinned on grinding papers under water to the thickness of about 0.1 mm. Final polishing was made electrolyticaly. Dislocation structures were observed by Philips CM 20 transmission electron microscope (TEM).

3. Results

3.1. Mechanical properties

Cyclic hardening softening curves in a wide interval of plastic strain amplitudes are shown in Fig. 1. Initial cyclic hardening for medium and high plastic strain amplitudes is followed by cyclic softening for all the amplitudes. The decrease of the stress amplitude with the logarithm of loading cycles is close to linear, i.e. the softening rate decreases with the inverse of the number of loading cycles (d| /dN 1/N ). Only for the highest plastic strain amplitude the tendency to saturation is apparent. Cyclic stress strain curve was drawn using the stress amplitudes in the half-life if the specimen failed or in the end of cycling for unbroken specimens. Fig. 2 shows the experimental points in double logarithmic plot. The usual type of the power law
b |a = Kbm n ap

Fig. 1. Cyclic hardening softening curves in constant plastic strain amplitude cycling (dotted curve separates the initial region before the desired plastic strain amplitude was reached).


Fig. 2. Cyclic stress strain curve and its approximation by power law in two domains. Table 1 Fatigue hardening coefcient and exponent evaluated in three domains of plastic strain amplitude Interval of map 10-5 = map = 102 10-5 = map = 103 10-3 = map = 10-2 Kb (MPa) 725 621 985 nb 0.081 0.065 0.134

does not t the experimental data and two domains with different slopes of the cyclic stress-strain curve can be distinguished. Table 1 shows parameters Kb and nb found in each interval of plastic strain amplitude evaluated using least squares tting.

3.2. SEM obser6ations

The development of surface slip markings resulting from the localization of the cyclic plastic strain was observed using direct observation in the SEM. The bands are well developed already early in the life. Fig. 3 shows the surface of the specimen cycled with map = 1 10 4 for 20 000 cycles, which is approximately 5%


T. Kruml, J. Pola k / Materials Science and Engineering A319 321 (2001) 564 568

along a single crystallographic plane. This observation is in accordance with the properties of dislocations in the b.c.c. lattice which can easily cross-slip. The typical thickness of the band at 5% of the fatigue life is around 0.5 mm but the band is as thin as 100 nm in the earliest stages of its development. The detailed view of the bands in Fig. 3 shows that the bands consist of extrusions, sharp intrusions and even nuclei of the microcracks.

3.3. Obser6ation of dislocation structures

Dislocation structures were studied in a virgin specimen, in a specimen cycled for 10 cycles at map = 1 10 3 and in specimens cycled with map = 5 10 5, 2 10 4, 1 10 3 and 5 10 3 up to fracture. The material in an annealed state contained low, but well detectable density of dislocations belonging to various slip systems. Majority of them were screw in character and formed subgrain boundaries. Two types of dislocation structures were found.

Fig. 3. Surface slip bands in specimen cycled at map = 1 10 4 up to 5% of the fatigue life. The mosaic-like background is due to electrolytic polishing.

Fig. 4. Subgrain boundary in a specimen cycled with map = 2 10 4 for N = Nf = 303 280, g = [010].

3.3.1. Dislocation structures formed in low plastic strain amplitude loading (map = 5 10 5 and 2 10 4) No clear spatial dislocation arrangement was formed in the specimens tested at low loading levels. Although the dislocation density was rather high, the microstructure is qualitatively similar to the one in the virgin material. Majority of dislocations are screw in character and form subgrain boundaries. An example of a subgrain boundary produced by the interaction of screw dislocations with two different Burgers vectors is shown in Fig. 4. The specic contrast producing a sharp tip image on one system of dislocations arises at locations where they dislocation of the rst slip system are traversed by dislocations of the second slip system. Dislocations of the second system are invisible in Fig. 4 under the present diffraction condition. Substantial amount of dislocations was found in the interiors of subgrains. At least two slip systems are activated in this low amplitude loading. 3.3.2. Dislocation structures formed in high plastic strain amplitude loading (map = 1 10 3 and 5 10 3) Cycling at high loading levels results in total rearrangement of the initial structure. Wall structure dominates the microstructure (Fig. 5). Since several slip systems are activated, the walls are usually produced by the interaction of dislocations from two different slip systems, which results in the formation of more or less regular labyrinth structure. The dislocation density in channels, as shown in Fig. 5, is generally high. However, areas in the form of a band with thickness of about 1 mm with substantially lower dislocation density were also observed (see the left part of Fig. 5). In the specimen cycled with the highest plastic strain ampli-

Fig. 5. Wall structure and a band with low dislocation density in the channels (PSB) in a specimen cycled with map = 1 10 3, N = Nf = 29 440, g = [010].

of the fatigue life. Macroscopically, the bands are nearly parallel (Fig. 3). Closer observation reveals, however, that the bands are wavy, i.e. they do not lie

T. Kruml, J. Pola k / Materials Science and Engineering A319 321 (2001) 564 568


tude (map = 5 10 3) the cell structure (Fig. 6) was most typical.

These wall segments are formed in a band and they are almost regularly spaced.

3.3.3. E6olution of dislocation structure with the number of cycles In order to understand the phenomenon of cyclic softening, the dislocation structure in a specimen cycled with map = 1 10 3 for 10 cycles, i.e. to the maximum of cyclic stress, was studied. High density of screw dislocations from several slip systems is produced. In the majority of grains, no traces of further rearrangement to the spatial dislocation structures were found. However, in some places the nuclei of walls have been already formed. The structure in such a grain is shown in Fig. 7. Two systems of screw dislocations can be identied in this Figure. Short, not well condensed wall segments are formed in the direction which bisects the obtuse angle between two systems of screw dislocations.

4. Discussion The simultaneous measurement of the cyclic stressstrain response and the study of the internal dislocation structures and surface relief in ferritic stainless steel revealed two domain of plastic strain amplitude in which the mechanical behavior and internal structure differ appreciably. In low amplitude domain (map B 1 10 3) the character of the dislocation arrangement does not differ qualitatively from that in the non-deformed material, only the dislocation density increases with the increase of the plastic strain amplitude. Since the effective stress represents an important fraction to the total stress amplitude the cyclic hardening exponent is low. In high amplitude domain (map \ 1 10 3) complete dislocation rearrangement takes place. Secondary wall and cell structures are formed due to the interaction of two systems of dislocations. The internal stress component becomes more important than in low amplitude domain and the cyclic hardening exponent increases. In spite of the different character of the dislocation arrangement in high and low amplitude domain cyclic softening has similar character in the whole interval of plastic strain amplitudes. The stress amplitude decreases approximately linearly with the logarithm of loading cycles. The surface observations show inhomogeneous distribution of the cyclic plastic strain. Also observations of the internal structure indicate the formation of the specic wall structures in the irregular bands early in the fatigue life. Both these observations suggest that the redistribution of the cyclic plastic strain and its localization into the bands of intensive cyclic slip (PSBs) is the source of intensive cyclic softening. The intensity of the softening is larger in comparison with austenitic stainless steels (f.c.c. structure) where only stabilized behavior or hardening (for high amplitudes) is found [12]. The reason for high softening rate can be sought in specic properties of dislocations in b.c.c. lattice. The edge segments are mobile while the plastic deformation rate is determined by the mobility of screw segments. As revealed by electron microscopy observations, already in cycling with the small amplitudes two slip systems can be active within one grain. The dislocations of these two systems can react and create low energy congurations. These low energy congurations are found as early as in 10 cycles in cycling with map = 1 10 3. The cyclic strain is concentrated into the bands of easy cyclic slip and the stress amplitude decreases both in the bands and in the matrix.

Fig. 6. Cell structure in a specimen cycled with map = 5 10 3, N = Nf = 1500, g = [110].

Fig. 7. Onset of wall formation in a specimen cycled with map = 1 10 3, N = 10, g = [010].


T. Kruml, J. Pola k / Materials Science and Engineering A319 321 (2001) 564 568

5. Conclusions Long-term cyclic softening characterizes cyclic straining of ferritic stainless steel in a wide domain of amplitudes. Intensity of softening decreases logarithmically with the number of cycles. Two domains on the cyclic stress strain curve correspond to two different types of internal dislocation structure. Cyclic softening can be related to the localization of the cyclic strain into softer bands (PSBs). The embryos of these bands can be detected already in the early stages of cycling. The localized plastic strain produces the bands of extrusions and intrusions on the surface.

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Acknowledgements The authors acknowledge the support of the grant No. A2041704 of the Grant Agency of the Academy of Sciences of the Czech Republic and grant No 106/97/P027 of the Grant Agency of the Czech Republic.