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Materials Science and Engineering A 415 (2006) 104117

The low-cycle fatigue, deformation and final fracture behaviour of an


austenitic stainless steel
Duyi Ye a,b, , Saburo Matsuoka b , Noburo Nagashima b , Naoyuki Suzuki b
a Department of Mechanics, Zhejiang University, Hangzhou 310027, China
b National Institute for Materials Science, 1-2-1, Sengen, Tsukuba-Shi, Ibaraki 305-0047, Japan
Received in revised form 31 August 2005; accepted 20 September 2005

Abstract
The low-cycle fatigue (LCF) behaviour of SUS304-HP austenitic stainless steel was investigated systematically using tension-compression
cycling under fully reversed total strain amplitude control conditions at room temperature in laboratory air. In addition to tests at constant strain
amplitudes, incremental step tests (IST) were also carried out. Cyclic stress response, during companion specimen tests (CST), revealed combinations
of a variable cyclic hardening, stable behaviour and softening, depending on the applied cyclic strain amplitude, while during incremental step tests
it exhibited cyclic hardening character at all strain levels. Microstructure observations using optical and transmission electron microscopy (TEM)
revealed that with increasing total strain amplitudes the slip band density increased and the dislocation structure changed from a planar array to
a more cellular-like structure. Cyclic deformation-induced austenite/martensite transformation was observed at higher cyclic strain amplitudes.
The change in microstructures during cycling is responsible for the fatigue hardening/softening behaviour of the material. The SEM micrographs
revealed that at low-strain amplitudes the inclusion-type nucleation occurred near the surface, while at the higher strain amplitudes crack initiation
characterized by cleavage cracking occurred not only near the surface but also in the interior of the specimen. Linear or single-slope behaviour
was seen both in cyclic stressstrain and Coffin-Mason plots. Masing cyclic stressstrain behaviour was presented only in the IST method but not
in the CST method.
2005 Elsevier B.V. All rights reserved.

Keywords: Low-cycle fatigue; Mechanical behaviour; Microstructure; Fracture feature

1. Introduction Despite the fact that low-cycle fatigue behaviour of type 304
stainless steel has been investigated for many decades and there
SUS304-HP is an improved version of type 304 austenitic exists a considerable literature on this topic at present [14],
stainless steel through the addition of nitrogen (N) element in relative limited amount of information on LCF behaviour of
its composition for purpose of enhancing the corrosion resis- SUS304-HP stainless steel is available. In earlier studies [5,6] on
tance and mechanical properties. This alloy is currently being the influence of nitrogen on fatigue properties of lower alloyed
used in industrial installations, such as petrochemical plants, austenitic stainless steels, it has been indicated that nitrogen as
electric-power generating stations and process plants as pip- an alloy element is capable of enhancing cyclic softening at
ing and structural material. In these applications, the compo- low-strain amplitude but causing hardening at the higher strain
nents of the structures are often subjected to repeated thermal amplitudes. The addition of nitrogen increased the low-cycle
stresses as a result of temperature gradients, which occur on fatigue lifetime of austenitic stainless steels [7,8]. The pro-
heating and cooling during startups and shutdowns or during cess behind improved fatigue properties is considered to be an
variations in operating conditions. Therefore, resistance to low- increased planarity in the slip mode, suppressing cross slip and
cycle fatigue (LCF) is an essential requirement in the design of promoting slip reversibility [7]. On the other hand, nitrogen was
these structures and components against failure under dynamic also found to play an essential role in stability of the austenite.
loading. Addition of nitrogen as an interstitial element favours the for-
mation of stacking faults and the formation of martensite during
straining, which reduces crack growth and leads to rapid hard-
Corresponding author. ening, i.e. it increases the resistance to plastic flow [911]. It
E-mail address: duyi ye@zju.edu.cn (D. Ye). was also indicated [12] that the effect of martensite formed on

0921-5093/$ see front matter 2005 Elsevier B.V. All rights reserved.
doi:10.1016/j.msea.2005.09.081
D. Ye et al. / Materials Science and Engineering A 415 (2006) 104117 105

LCF life depended on the amount of martensite present, strain to determine the cycle stressstrain curve (CSSC). In this case,
amplitude, grain size and whether crack initiation or propagation a specimen was subjected to repeated strain blocks in which the
controlled fatigue life at a given strain amplitude. In one study strain amplitude increased from 0.2% linearly up to 1.2%, and
[13], the LCF properties deteriorated on martensite formation, then decreased. The IST was also run until the specimen failed.
owing to more crack initiating sites becoming available. From During testing, the load was continually monitored and hys-
earlier studies, it can thus be expected that the low-cycle fatigue teresis loops were recorded at appropriate intervals by means
behaviour of SUS304-HP stainless steel with a certain content of a personal computer with a data-collecting and analyzing
of nitrogen will be different from that of conventional type 304 software.
austenitic stainless steel without containing nitrogen content. The microstructures of the alloy after fatigue tests were
In this paper, low-cycle fatigue tests of SUS304-HP stain- examined by both optical microscopy (OM) and transmission
less steel were carried out at room temperature under total strain electron microscopy (TEM). Samples for microstructural
control using companion specimen test (CST) and incremen- analysis were prepared below the fractured surface in fatigue
tal step test (IST) methods, respectively. A detailed examina- failed specimens by cutting perpendicular to the tensile axils
tion of deformation microstructures and fracture features of the with a wire saw. The samples for OM were ground using emery
fatigue specimens cycled to failure at various strain amplitudes papers of various grinds from 230 to 600 grit, and then etched
was also performed. The low-cycle fatigue characteristics were for 30 s in a solution of 16 vol% of HNO3 , 32 vol% of HCl and
then discussed by means of competing and mutually interactive 50 vol% of glycerol at 313 K. Samples for TEM obtained from
influences of cyclic strain amplitude, concomitant mechani- thin slice with 0.3 mm thickness were mechanically thinned
cal response, intrinsic microstructural effects and dislocation- to 30 m, and then electropolished in a solution containing
microstructure interactions during cyclic straining. The main 5 vol% of perchloric acid and 55 vol% acetic acid, using a
purpose of the present work is to gain a more complete under- twin jet apparatus at a potential of 20 V and a temperature
standing of the low-cycle fatigue behaviour of SUS304-HP of 798 K. TEM examinations were performed on a HITACH
austenitic stainless steel, especially concerning the analytical H9000NA transmission electron microscope, operating
relationship describing its behaviour, so as to use it more effec- at 300 kV.
tively in practical structural designing against fatigue. The fractured surfaces of the fatigue failed specimens were
ultrasonically cleaned in trichloroethylene, and then observed
2. Experimental details using a low-magnification binocular microscope to locate rel-
evant feature, which were subsequently examined at higher
The material used for present investigation was SUS304-HP magnification with a JEOL JSM-T20 scanning electron micro-
austenitic stainless steel supplied in the form of a plate, 22 mm scope (SEM) to determine the predominant fracture mode and
in thickness. The plates were hot rolled at 1040 C for 0.2 h, to characterize the fine-scale topography of the fatigue fracture
followed by quenching in water. The nominal chemical compo- surface.
sition of the material in percentage weight is listed in Table 1.
Specimens used in the low-cycle fatigue tests were cylindri- 3. Results
cal, 6.0 mm in diameter and 14 mm in the gauge-length section.
Fully reversed, pushpull and total strain amplitude controlled 3.1. Initial microstructure and tensile properties
fatigue tests were performed at room temperature in an ambient
air using a closed-loop servohydraulic testing machine (Shi- The microstructure of the SUS304-HP stainless steel in the
madzu). A triangular strain waveform with zero mean strain as-heat treated conditions, as shown in Fig. 1, consisted of ran-
(R = 1) at a constant total strain rate of 5 103 S1 was domly oriented grains with a few annealing twins. Both the
used. The tests were continued until fracture, with the strain grain and twin boundary were covered with discrete carbide
amplitude limits lying between 0.30 and 2.0%. The test fre- particles. The heat-treatment conditions mentioned previously
quency (f) at a certain total strain amplitude could be defined by result in an equiaxed grain size, measured by the conven-
the following formula, f = /(4a ), where a is the total strain tional linear intercept method, of approximate 88 m (twins
amplitude. The incremental step test method was also employed not taken into account). Fig. 2 shows a transmission electron
microscopy micrograph of the material in the same condi-
Table 1
tion, which reveals that the dislocation structure in the ini-
Chemical composition (wt%) of SUS304-HP austenitic stainless steel tial condition consists of pinned dislocation lines and small
loops with low-dislocation density. Both optical microscopy
C 0.06
Si 0.45
and transmission electron microscopy observations indicate
Mn 0.81 that, in the undeformed condition, there was no metallo-
S 0.006 graphic evidence of austenite/martesitic transformation in the
P 0.029 material.
Cr 18.19 The tensile properties of the present material are summa-
Ni 8.64
N 0.052
rized in Table 2. The results reported are the mean values based
Fe Bal. on multiple (three) tests. The yield strength ( ys ) defined as
the stress corresponding to a plastic strain of 0.2% is 275 MPa.
106 D. Ye et al. / Materials Science and Engineering A 415 (2006) 104117

Fig. 3. Cyclic stress response curves.

Fig. 1. Optical micrograph of SUS304-HP stainless in the as-heat treated con- 3.2. Low-cycle fatigue behaviour
ditions.

3.2.1. Cyclic stress response curve


The cyclic stress response curve obtained by plotting the
cyclic stress amplitudes, determined by averaging the maximum
tensile and compressive stress in a hysteresis loop versus the
number of cycles in a total strain-controlled fatigue test, illus-
trates the path by which the material arrives at the final cyclic
flow stress level [14]. Fig. 3 shows the cyclic stress response
curves of the SUS304-HP steel at five different total strain ampli-
tudes. As can be seen, the cyclic stress response is dependent on
strain level and can be generally characterized as the following
three circumstances, i.e. (1) at strain amplitudes less than 0.6%,
the material displayed very small initial hardening followed by
a progressive softening, and then a saturation up to the final
failure, (2) at strain amplitude of 0.9%, the initial mild harden-
ing was followed by a region of nearly stable stress response,
and then a pronounced secondary hardening, which persisted
until fracture and (3) at strain amplitudes larger than 1.2%, the
Fig. 2. Dislocation structure of SUS304-HP stainless steel in the as-heat treated material exhibited very rapid strain hardening almost without
conditions. reaching its saturated values till final fracture. In order to make
comparison of the relative magnitude of the initial hardening,
The ultimate strength ( ult ) is 618 MPa. The large difference which occurs at the different strain amplitudes, a simple expres-
between the yield strength and ultimate strength indicates that sion for description of the degree of hardening (H) is given by
this material exhibits a significant amount of work hardening the following equation [15],
during monotonic deformation. The elongation to failure and asat a1
reduction in area were 68 and 82%, respectively. These tensile H= (1)
a1
properties reveal that SUS304-HP stainless steel has medium
strength and high ductility. where a1 and asat are the stress amplitude at first cycle and the
saturated stress amplitude, respectively.
The degree of cyclic strain hardening (H) plotted as a function
Table 2 of applied strain amplitudes (a ) is shown in Fig. 4. This figure
Mechanical properties of SUS304-HP stainless steel
indicates that with increasing applied strain amplitude the cyclic
0.2% proof stress, ys (MPa) 275 strain hardening occurring in the material increases linearly. The
Ultimate tensile strength, ult (MPa) 618 strong dependence of cyclic strain hardening on imposed strain
Elongation, (%) 68
Reduction of area, f (%) 82
amplitude was also reported in other austenitic stainless steels,
such as types AISI 304L and AISI 316 [11,16].
D. Ye et al. / Materials Science and Engineering A 415 (2006) 104117 107

Table 3
Cyclic stress response and fatigue life data of the SUS304-HP stainless steel
t /2 Values at N = 0.5Nf Nf

e /2 p /2 /2

0.003 0.00121 0.00178 235.5 132400


0.004 0.0014 0.0026 268.8 17960
0.005 0.00152 0.00348 293 23400
0.006 0.00168 0.0043 323.8 4680
0.009 0.00218 0.00682 419.0 1249
0.01 0.00236 0.00763 455 753
0.012 0.00272 0.00927 522.1 506
0.015 0.00305 0.0119 583.4 260
0.02 0.0032 0.0168 609.1 165

features especially at the lower strain amplitudes. In the case of


the IST, the material exhibits cyclic hardening character at all
strain amplitudes investigated. The above results suggest that for
SUS304-HP austenitic stainless steel, the cyclic stress response
depends greatly on the type of loading or the cyclic-strain his-
Fig. 4. Dependence of the degree of cyclic strain hardening on imposed strain tory applied to the specimen in additional to the imposed strain
amplitude. amplitudes.

To assess the effect of the type of loading on cyclic harden- 3.2.2. Cyclic stressstrain curve and Manson-Cofn plot
ing/softening behaviour of SUS304-HP stainless steel, the cyclic The results of low-cycle fatigue tests for the present material
response for the incremental step test method was determined, are reported in Table 3. The elastic strain amplitude (ea ), plastic
in which the stress amplitude responses at strain amplitudes of strain amplitude (pa ), total strain amplitude (ta ) and saturation
0.4, 0.6, 0.9 and 1.2% in each strain block are plotted as a func- stress amplitude ( a ) in this table are deduced from the hysteresis
tion of fraction of block (bn /bf ), as shown in Fig. 5. In this loops corresponding to half of the total number of cycles to
figure, the cyclic stress response determined by the companion fracture.
specimens test method, shown in Fig. 3, is also presented for Fig. 6 shows the cyclic stressstrain curves of the material
comparison purpose, where the stress amplitude during strain determined by the CST and IST methods, respectively, where the
cycling is plotted as a function of fraction of life (N/Nf ). It is values of stress and strain amplitudes for the IST method were
found from this figure that the cyclic stress response determined taken at half of the total number of strain blocks to fracture. As
by the above two methods exhibit quite different characteristic a comparison, the monotonic stressstrain curve (MSSC) of the
material is also presented in this figure. It is seen that both the

Fig. 5. Comparison of cyclic stress response curves determined by the CST and Fig. 6. Cyclic stressstrain curves (CSSCs) determined by the CST and the IST
the IST methods. methods and monotonic stressstrain curve (MSSC).
108 D. Ye et al. / Materials Science and Engineering A 415 (2006) 104117

CSSCs determined by the above two methods and the MSSC


exhibit a straight line in the bilogarithmic plot, from which a
high-strain-hardening capacity in the CST compared with that in
the IST and the monotonic tensile test is inferred. This observa-
tion indicates that for the SUS304-HP stainless steel the capacity
for the work hardening inherent in the material greatly depends
on the type of loading in addition to the imposed strain levels.
The incomparability of the CSSCs determined by the CST and
the IST methods, as presented in Fig. 6, suggests that for the
material chosen there is no possibility of using one specimen
to determine the cyclic stressstrain curve. On the other hand,
it is also easily deduced from the relative positions between
the CSSCs and MSSC, shown in Fig. 6, that in the CST the
material exhibits cyclic strain softening at low-plastic strain
regions (pa 0.2%) but cyclic hardening at the high-plastic
strain regions (pa 0.2%), while in the IST the material exhibits
cyclic hardening over the range of strain amplitudes investigated.
This deduction is in accordance with the dependence of cyclic
stress response on applied strain amplitude, as shown in Fig. 3, Fig. 7. Strain amplitude-life plot.
and on the type of loading, as shown in Fig. 4.
A cyclic stressplastic strain relationship of the form [17],
 The test data of ea , pa , ta and 2Nf listed in Table 3 are plot-
a = K (ap )n (2) ted on a bilogarithmic scale in Fig. 7. The data of both elastic
and plastic strain components showing a linear relationship on
where K is the cyclic strength coefficient and n the cyclic strain-
a loglog plot suggests that Eq. (3) can be used to determine
hardening exponent, was fitted by the least squares technique for
the fatigue behaviour. The values of low-cycle fatigue empirical
the data presented in Table 3. The derived values of K and n for
parameters that satisfy Eq. (3), determined using least-square
both the CST and IST methods are listed in Table 4, in which the
analysis are summarized in Table 5. It is seen from this table
material constants (K and n) obtained in the monotonic tensile
that the value of fatigue parameter (b) is 0.17. This value is
test are also given for comparison purpose. It is noted from
more negative than that for the stable materials in which b ranges
Table 4 that the cyclic strain-hardening exponent (n ) determined
from 0.05 to 0.15 [18]. The fatigue ductility exponent (c) is
in the CST is higher than that determined in the IST almost by
0.346, which is within the generally observed range (0.7 to
a factor of 2.5 and larger than the strain hardening exponent (n)
0.2) for a large number of monolithic alloys and their com-
obtained in the monotonic tensile test.
posite counterparts [19,20]. The fatigue ductility coefficient (f )
The variation of fatigue life, in terms of number of reversals
is 0.105, which does not accord with the monotonic ductility as
to failure (2Nf ), with elastic strain amplitude (ea ), plastic strain
measured by the elongation to failure (f ) of 1.71. It has been
amplitude (pa ) and total strain amplitude (ta ) is analyzed on
indicated that f was lower than f by a factor of 220, depending
the basis of the strain-life relationship proposed by Basquin and
on the material condition and the testing parameters employed
Coffin-Manson, which can be written in the form [17],
[1]. Such an unsatisfactory correlation between f and f has also
f been reported by Hennessy et al. [21] and by Landgraf [18]. The
a = ae + ap = (2Nf )b + f (2Nf )c (3) inferior cyclic ductility for the present material is ascribed to
E
local stress (and strain) concentrations and deformation char-
where f , b, f and c are the fatigue strength coefficient, fatigue acteristics of the microstructure features during fully reversed
strength exponent, fatigue ductility coefficient and fatigue duc- cyclic straining.
tility exponent, respectively. As shown by Morrow and Tuler [22] through energy
arguments, the fatigue strength exponent (b) and fatigue
Table 4 ductility exponents (c) can also be determined from the cyclic
Values of n and K determined by the CST and IST methods
Monotonic tensile test
n 0.08 Table 5
K 484 Values of f , b, f and c
CST
f (MPa) 1415.1
n 0.336
b 0.17
K 3722
b = n /(1 + 5n ) 0.125
IST f 0.105
n 0.13 c 0.346
K 933 c = 1/(1 + 5n ) 0.37
D. Ye et al. / Materials Science and Engineering A 415 (2006) 104117 109

Fig. 8. Stressstrain hysteresis loops plotted with matched lower tips: (a) the CST method; (b) the IST method.

strain-hardening exponent (n ), The expression for calculating the plastic stain energy for a
non-Masing-type material was developed by Jhansale and Top-
n 1 per [25] and can be written as,
b , c (4)
1 + 5n 1 + 5n    
1n 2n
These calculated values are listed in Table 5 and exhibit Wp = (p ) + (0 p ) (6)
1+n 1+n
agreement with those found from the test. This indicates
that, as a first approximation, the empirical relationship (4) is where n is the exponent of the equation of the skeleton curve,
applicable for the case of the SUS304-HP stainless steel. p = (/2E0 )1/n , and 0 represents the increase in the
proportional stress range due to non-Masing behaviour of the
3.2.3. Masing-type behaviour and cyclic plastic strain material.
energy From the tests data of SU304-HP stainless steel, the coef-
Tests were also carried out to determine whether SUS304- ficient n of Eq. (6), evaluated by a least squares technique, is
HP stainless steel exhibits Masing cyclic stressstrain behaviour 0.21. Note that the value of n is quite different from the cyclic
(or Masing-type behaviour) at room temperature. This prop- strain-hardening exponent n (see Table 4). The increase in the
erty is important for description of the hysteresis loop during proportional stress range, 0 , can be obtained from the cyclic
cycling. Fig. 8a and b shows the superimposed loops plotted stressstrain curve and is given by 0 = (/2) 60. The plas-
with matched lower tips for both the CST and IST methods. It is tic strain energy per cycle at half-life, determined by measuring
seen that the material exhibits Masing-type behaviour in the IST the area of the hysteresis loop and calculated from Eqs. (5) and
but does not follow an ideal Masing-type behaviour in the CST. (6), are reported in Table 6. It easily follows from this table that
According to Abdel-Raouf et al. [23], Masing-type behaviour the prediction precision of the plastic strain energy based on Eq.
could be determined using the Bauschinger strain (), defined as (6) has been improved greatly due to reckoning into the effect
the plastic strain in the reverse direction at 75% of the prestress in of non-Masing-type behaviour.
the forward direction. The Bauschinger strain () plotted against
plastic strain range (p ) is shown in Fig. 9. It follows from this
figure that for the case of IST the material exhibits Masing-type
behaviour, since Bauschinger strain () increased linearly with
cyclic plastic strain range (p ), while in the case of the CST
non-Masing-type behaviour could be inferred owing to the fact
that Bauschinger strain () increased with plastic strain range
(p ) in a parabolic manner after an initial linear region at low-
strain levels. The above two methods made the same predictions
of Masing-type behaviour for the material investigated.
It is known that for the material exhibiting a Masing-type
behaviour, the cyclic hysteresis energy per cycle Wp can be
calculated directly in terms of the cyclic stressstrain curve Eq.
(2), and can thus be expressed as [24],
 
1 n
Wp = p (5)
1 + n
where  (=2 a ) is the total stress range and p (=ap ) the
plastic strain range. Fig. 9. Bauschinger strain vs. plastic strain range.
110 D. Ye et al. / Materials Science and Engineering A 415 (2006) 104117

Table 6 Fig. 11b. In agreement with the observations of Bayerlein et al.


Comparison of experimental and theoretical values of plastic strain energy per [11] during cyclic deformation of AISI 304L stainless steel, a
cycle
direct austenite/martensite transformation must have occurred
a (%) Wp (MPa) Wp (MPa) Wp (MPa) in the austenitic matrix of the material within this strain ampli-
measured calculated according calculated according tude. At the high-strain amplitude (a = 2.0%), most of grains
experimentally to Eq. (5) to Eq. (6)
in the specimen contained two or more activated slip systems
0.40 2.03 1.42 1.88 and the interband spacing becomes smaller (see Fig. 12a). The
0.60 4.2 2.84 4.08 high-magnification micrograph (Fig. 12b) reveals the presence
0.90 8.8 5.83 8.44
1.2 14.8 9.91 13.84
of spatially distributed bands with different contrast. As sug-
2.0 30.8 21.12 29.05 gested by Botshekan et al. [16], these bands can be ascribed
to the presence of microtwins and martensite platelets. The
amount of austenite/martensite transformation in the austenitic
3.3. Deformation microstructure matrix further increases with strain amplitude (see Fig. 12c),
where martensite with an irregular blocky shape extended com-
The investigation of deformation microstructures was pletely across grains or as platelets arranged in bands was
focused on examining and understanding their physical correla- visible.
tion to low-cycle fatigue behaviour of the material presented The dislocation structures observed in specimens cycled to
in the previous section. Thus, the slip band and dislocation failure at three strain amplitudes are summarized in Figs. 1315.
structure developed in the fatigued specimens tested at three At a lower strain amplitude (a = 0.6%), the austenitic grains
strain amplitudes (a 0.6%, a = 0.9% and a 1.2%) that cor- show a progressive accumulation of dislocation arrays and pile-
respond to the three circumstances of the cyclic stress response ups of planar character, mainly correlated to a unique slip
curves shown in Fig. 3 and from now on referred to as low, plane within individual grains (Fig. 13a). These planar arrays
intermediate and high-strain amplitudes are examined. are formed by dissociated dislocations, clearly identified for
Figs. 1012 show typical optical micrographes taken from showing stacking fault contrast as observed in Fig. 13b. At
a deformed region of the specimens cycled to failure at three the intermediate strain amplitude (a = 0.9%), the dislocation
strain amplitudes mentioned above. At the low-strain ampli- structure was characterized by elongated and not fully devel-
tude (a = 0.4%) the grains generally contained a few slip oped cells (see Fig. 14). Both within and outside the cells,
bands and slip was restricted to one system of parallel {1 1 1} a number of dislocation loops and debris were observed. The
planes (Fig. 10). At an intermediate strain amplitude (a = 0.9%) poorly developed cells must be the result of dislocations from
increasing imposed strain amplitude results in the activation different slip systems interacting and trapping each other at
of new slip systems, a higher density and more uniform dis- intersecting regions, as suggested by Jin et al. [26]. At the
tribution, from grain to grain, of the slip bands (Fig. 11a). high-strain amplitude (a = 2.0%), the cellular dislocation struc-
Meanwhile, the martensitic phase appeared as thin parallel indi- tures or subgrains were fully developed and densely clustered
vidual striations in the austenitic grains, as shown by arrows in in the majority of grains, as has been observed in Fig. 15a. The
regions between the dislocation cells are almost entirely dislo-
cation free. In some grains, the cellular structure is penetrated
by individual striations having parallel orientation (Fig. 15b).
In analogy with similar striations observed by Botshekan et al.
[16], after unidirectional cyclic straining, these striations can
be ascribed to the presence of microtwins and/or martensite
platelets.

3.4. Cyclic fracture features

Examination of the fracture surface of the low-cycle fatigue


specimens was performed: (a) at low magnification to identify
the fatigue and final fracture (overload) regions and (b) at higher
magnifications to identify regions of crack initiation and early
crack growth in the fatigue region, and also to identify the fine-
scale fracture features in the overload region.
Figs. 1618 show representative micrographs of the fracture
surfaces features of the specimens cycled to failure at low, inter-
mediate and high-strain amplitudes, respectively. At the low-
cyclic total strain amplitude (/2 = 0.4%), the crack initiated
near the surface and propagated inward, leaving a distinct region
Fig. 10. Optical micrograph showing slip band features in the fractured speci- of crack propagation, which appeared as alternating furrows and
men tested in LCF at a = 0.4%. ridges or strips of steps (Figs. 16a and b). High-magnification
D. Ye et al. / Materials Science and Engineering A 415 (2006) 104117 111

Fig. 11. Optical micrographes in the fractured specimen tested in LCF at a = 0.9% showing: (a) slip band features; (b) morphologies of martensite.

observations of the crack nucleation or formation region early growth region (Fig. 16d) revealed a crystallographic (stage
revealed the crack initiation to occur at inclusions near the sur- I) morphology of crack growth characterized by arrangements of
face (Fig. 16c). The inclusion-type nucleation can be understood wavy striations that have steps intersection at right angles. The
as cyclic slip localization due to stress-concentration at the inclu- arrangements of steps are comparable to brittle striations. The
sion, leading to either decohesion of the inclusionmatrix inter- overload region (Fig. 16e) comprised of microscopic voids of a
face or cracking of the inclusion [17]. Observations of the crack variety of sizes and shallow dimples indicating the highly ductile

Fig. 12. Optical micrographes in the fractured specimen tested in LCF at a = 2.0% showing: (a and b) slip band features; (c) different morphologies of martensite.
112 D. Ye et al. / Materials Science and Engineering A 415 (2006) 104117

Fig. 13. TEM micrographs in the fractured specimen tested in LCF at a = 0.6% showing: (a) a planar array of dislocation structures; (b) stacking faults.

ation or formation region revealed the presence of fatigue slip


bands and cyclic cleavage facets (Fig. 17c). The region of early
crack growth showed distinct evidence of crystallographic (stage
I) crack growth prior to propagation of the crack along a plane
normal to the stress axis (stage II), as shown in Fig. 17d. In
analogy with what was observed at the low-strain amplitude,
the sudden fracture region also exhibits high-ductile character-
istic (Fig. 17e). At the high-strain amplitudes (a = 1.2%), the
crack initiated not only near the surface but also in the interior
of the specimen (Fig. 18a and b). Higher magnification obser-
vations of the crack nucleation region revealed that cleavage
fracture was characteristic of fatigue crack nucleation at this
strain amplitude (see Fig. 18c). An example of deformation twins
as nucleation sites of cleavage fracture is shown in Fig. 18d. The
crack nucleation of this type is termed direct cleavage crack-
ing, in contrast to that initiated by shear, indicates thereby that
Fig. 14. TEM micrographs showing loose and incomplete dislocation cell struc- shear cracking is not the only mechanism for crack nucleation
ture in the fractured specimen tested in LCF at a = 0.9%. at the higher strain amplitudes. Observations of the regions of
transgranular fracture (Fig. 19e) revealed the fatigue striations to
nature. At the intermediate strain amplitude (/2 = 0.9%) the be covered with finer striations, which are indicative of repeated
fracture features on a macroscopic scale were similar to those plastic deformation occurring in a single cycle and accompa-
observed at the lower strain amplitude, as shown in Fig. 17a. nied by local secondary cracks along striations. High magni-
Microcracks originated from the specimen surface was also char- fication observation of the sudden fracture regions (Fig. 19f)
acteristic of fatigue crack nucleation at this strain amplitude (see revealed microscopic features indicative of classic ductile
Fig. 17b). Higher magnification observations of the crack nucle- fracture.

Fig. 15. TEM micrographs in the fractured specimen tested in LCF at a = 2.0% showing: (a) well-developed dislocation cell structure; (b) cellular structure penetrated
by individual striations with parallel orientation.
D. Ye et al. / Materials Science and Engineering A 415 (2006) 104117 113

Fig. 16. (ae) Macroscopic fractograph and SEM micrographs of the fracture surface in the specimen tested in LCF at a = 0.4%.

4. Analysis and discussion [27], an increase in slip band density is responsible for the hard-
ening in austenitic steels. To verify this suggestion, specimens
The micromechanisms responsible for the cyclic stress tested at different total strain amplitudes were also examined
response during low-cycle fatigue are dependent on the for the present material. The number of slip bands per grain
microstructure and strain amplitude [17]. In the as-heat treated was divided by the grain diameter in a direction perpendicu-
conditions of SUS304-HP stainless steel, the initial microstruc- lar to the slip bands to estimate the average slip band spacing.
ture comprises pinned dislocation lines and loops with low- About 5075 grains were counted for each specimen. Fig. 19
dislocation density (Fig. 2). During cyclic straining, the unpin- shows the dependence of slip band spacing on imposed strain
ning and multiplication of dislocations as well as the mutual amplitudes, in which a decrease in slip band spacing with an
interactions of dislocations and the interactions of dislocations increase in the applied strain amplitude was observed. Thus,
with grain boundaries increases the resistance to plastic defor- consistent with earlier studies [27,28], it can be inferred that
mation, which is responsible for the observed initial hardening in an increase in the degree of cyclic strain hardening with strain
the cyclically deformed material. According to Lerch and Gerod amplitude for the present material, as shown in Fig. 4, can be
114 D. Ye et al. / Materials Science and Engineering A 415 (2006) 104117

Fig. 17. (ae) Macroscopic fractograph and SEM micrographs of the fracture surface in the specimen tested in LCF at a = 0.9%.

related to the number of slip bands and slip systems activated in transformation [16,21]. Therefore, after initial cyclic hardening,
the cyclically deformed specimens. Since the material studied the stress response of the present material is governed by two
here is quasi-stable at room temperature due to addition of nitro- competitive processes, namely dynamic recovery (i.e. formation
gen, it underwent a deformation-induced austenitic/martensitic of cells and subgrains) and defomation-induced martenstic trans-
transformation during cyclic straining. Numerous investigations formation. The formation of cells and subgrains due to recovery
[913] have shown that the formation of martensites during mechanisms leads to an increase in the mean path for disloca-
cyclic loading strongly affects the fatigue mechanical behaviour tions, which favours cyclic softening [1], whereas the formation
of various types of steels. Magnetic measurements on the frac- of martensite by strain-induced processes drastically increases
ture surface of fractured specimens after the LCF deforma- the resistance to plastic flow that promotes cyclic hardening of
tion showed that the martensite content had increased with the the material [11]. According to TEM observations at low-strain
applied total strain amplitude [10]. The measurement of the vol- amplitudes, the saturation dislocation structures in the deformed
ume fraction of martensite during fatigue tests also documented specimen displayed a planar-array dislocation configuration
that a direct relation exists between hardening and martensitic (Fig. 13a). Both OM and TEM examinations revealed no marten-
D. Ye et al. / Materials Science and Engineering A 415 (2006) 104117 115

Fig. 18. (af) Macroscopic fractograph and SEM micrographs of the fracture surface in the specimen tested in LCF at a = 1.2%.

site formation in austenitic grains tested at this strain amplitude. compensate for the softening effect associated with dislocation
This agrees with the findings of Baudy and Pineau [10] con- cellular structure, the material exhibits a saturation character as
cerning the critical total or plastic strain amplitude, which must has been observed in the cyclic stress response curves (Fig. 3),
be achieved in order to induce martensite formation in cyclic which is followed by secondary hardening as a result of the fact
straining. Consequently, at low-strain amplitude, the progres- that the volume fraction of strain-induced martensite transfor-
sive softening process after initial cyclic hardening is attributed mation further increased with the increasing number of straining
to the formation of a dislocation configuration that bears the plas- cycles. At high-strain amplitudes, the cumulation of the cyclic
tic strain more easily [17]. At the intermediate strain amplitude plastic strain leads to a continuous increase in the density of shear
austenite/martensite transformation takes place and the amount bands, and thus in the density of sites for strain-induced nucle-
of this transformation increases with an increasing number of ation of martensite (see Figs. 12c and 15b). In other words, more
cycles, as shown in Fig. 11b. Meanwhile, the tendency to form a martensite is formed with a less number of cycles in this case. As
dislocation substructure characterized by a developing cell struc- a result, the material displayed continuous strain hardening up
ture containing low-dislocation density/ill-defined cell walls to failure without displaying an intermediate stage of stress sat-
(Fig. 14) suggests localization of deformation in the material, uration at the higher strain amplitudes (see Fig. 3). On the other
which results in less stress for sustaining a given strain ampli- hand, the formation of more martensite also leads to more crack
tude, namely softening. Thus, when an increase of the resistance initiating sites in the fatigued specimen at high-strain amplitude,
to plastic deformation resulting from formation of martensite can which has been exhibited in the fatigue fracture (see Fig. 18ad).
116 D. Ye et al. / Materials Science and Engineering A 415 (2006) 104117

5. Conclusions

The experimental results on the room-temperature low-cycle


fatigue behaviour, deformation microstructures and fracture fea-
tures of the austenitic stainless steel SUS304-HP reported in this
paper support the following conclusions:

(1) Cyclic stress response, during companion specimen tests,


revealed combinations of a variable cyclic hardening, sta-
ble behaviour and softening, depending on the applied cyclic
strain amplitude, while, during incremental step tests, exhib-
ited hardening character at all strain levels. In the case of the
CST, the degree of cyclic strain hardening increases almost
linearly with increasing strain amplitude.
(2) The CSS curves obtained by the CST and IST methods
exhibits different characteristic features. The CST, com-
pared to the IST, gives a higher slope of the CSSC or a
higher strain hardening capacity at all strain amplitudes.
Fig. 19. Variation of slip band spacing with strain amplitude. Therefore, in the case of the present material, there is no
possibility of using one specimen to determine the cyclic
stressstrain curve.
The sensitivity of the cyclic stress response to the type of (3) The fatigue lifetime shows single-slope behaviour in both
loading or the imposed strain history, as shown in Fig. 5, was Basquin and Cofffin-Manson diagrams.
also reported in other austenitic stainless steels, such as AISI (4) Masing cyclic stressstrain behaviour was presented only in
316L and AISI 446 [29], and was explained as a result of the the IST method but not in the CST method. The prediction
strong evolution of dislocation structures and nucleation of the precision of the cyclic plastic strain energy was improved
deformation-induced martensitic transformation during fatigue greatly due to reckoning into the effect of non-Masing-type
testing. Since the dislocation structure built up in the IST was behaviour in terms of the modified equation developed by
mostly characteristic of the highest strain amplitude in the strain Jhansale and Topper [25].
block and remained practically that of the highest strain ampli- (5) Observations of fatigue-related microstructures revealed
tude throughout the block [12], both the saturation dislocation that with increasing total strain amplitude the slip band den-
structure and the martensite transformation in the present mate- sity increased and the dislocation structure changed from
rial can be expected to be formed at early stages of strain blocks a planar dislocation array to a more cellular-like struc-
due to the fact that the highest strain amplitude occurred in ture. A strong tendency of the cyclic deformation-induced
each strain block. In other words, the material remained prac- austenitic/martensitic transformation was observed in the
tically similar regardless of stress amplitudes in the IST. As a austenitic matrix at higher cyclic strain amplitudes.
result, the material exhibits cyclic hardening in the IST even (6) The SEM examinations revealed that at low-strain ampli-
when the strain amplitude decreased within a block, as has been tudes the inclusion-type nucleation occurred near the sur-
observed in Fig. 5. In the CST, however, the dislocation structure face, while at high-strain amplitudes the crack initiation
was different at different strain amplitudes and more martensite characterized by cleavage cracking occurred not only near
formed at the high-strain amplitudes, which is responsible for the surface but also in the interior of the specimen.
the observed hardening/softening behaviour in the cyclic stress
response curves. The lower slope for the CSSC obtained by the Acknowledgements
IST as compared to that determined by the CST, as shown in
Fig. 6, is in agreement with observations by Nystrom et al. [30] The first author would like to express his sincere thanks
and Zhong et al. [31] in AISI 316L and AISI 310 types of stain- to Dr. Akihiko OHTA, the former host researcher of the first
less steel. It is likely that this general difference in slope between author, who provided financial assistance through 2001Y JSPS
the two methods is caused by differences in the developing dis- Postdoctoral Fellowship under Grant PB01021. He also wishes
location structure during the IST and CST. This difference of to acknowledge the National Institute for Materials Science
the microstructure induced by the two methods can be used to (NIMS), Japan, for his appointment as a visiting researcher in
explain why Masing-type behaviour was seen in the IST but Materials Information Technology Center during February 1st,
not in the CST, for Masing-type behaviour is expected to be 2002 through January 31st, 2004.
present only for the cases where the microstructure does not
change appreciably [12]. In other words, the difference of the
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