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Engineering Fracture Mechanics 115 (2014) 241–254 Contents lists available at ScienceDirect Engineering Fracture

Contents lists available at ScienceDirect

Engineering Fracture Mechanics

journal homepage: www.elsevier .com/locate/engfracmech A fracture mechanics approach to interior fatigue crack

A fracture mechanics approach to interior fatigue crack growth in the very high cycle regime

Takeshi Ogawa a , 1 , Stefanie E. Stanzl-Tschegg b , , Bernd M. Schönbauer b , 2

a Aoyama Gakuin Univ., Dept. of Mechanical Engineering, Fuchinobe 5-10-1, Chuou-ku, Sagamihara-shi, Kanagawa 252-5258, Japan b University of Natural Resources and Life Sciences (BOKU), Peter Jordan Strasse 82, 1190 Wien, Austria

Sciences (BOKU), Peter Jordan Strasse 82, 1190 Wien, Austria article info Article history: Received 26 February

article info

Article history:

Received 26 February 2013 Received in revised form 18 October 2013 Accepted 2 November 2013 Available online 14 November 2013

Keywords:

Ultrasonic fatigue Cumulative damage Repeated two-step tests Fish-eye fracture Fatigue crack growth

abstract

Growth rates of optically dark areas (ODA) and fish-eyes (FE) were quantified in kHz- ultrasonic fatigue tests on SUJ2 and 17-4PH steels at constant and repeated two-step amplitudes. Sizes of ODAs and FEs depended on the stress intensity factor (SIF) range, and interior fatigue crack growth rates (FCGR) were slower than those of ‘‘long’’ cracks in air, suggesting vacuum as ODA growth environment. Repeated two-step tests on SUJ2 steel served to form beach marks so that, a quantification of ODA sizes, interior FCGRs and SIFs became possible. Additional FCGR measurements of long cracks in vacuum and comparable fracture morphologies allowed estimating the growth rates of ODAs and FEs in 17-4PH steel.

2013 Elsevier Ltd. All rights reserved.

1. Introduction

Due to the demand for longer fatigue lives in technical equipment and constructions, research on fatigue failure has at- tracted increased attention recently. Responding to this demand, material scientists continually develop new materials with improved fatigue properties, therefore also relying on exact fatigue failure measurements. As early as 1978, Schijve emphasized the importance of internally growing cracks in aluminum alloys and showed that the resulting fatigue lives were determined by such cracks growing in a vacuum under realistic loading conditions [1] . In the 1980s, research on the very high cycle fatigue (VHCF) properties of high-strength steels received a most important input, namely the detection of failures beyond the traditionally assumed fatigue limit in the regime of 10 6 –10 7 cycles [2,3] . More- over, under special conditions (i.e. material properties, surface condition, amplitude of loading, number of cycles, etc.) such VHCF failures were found to originate in the interior of the specimen, whereas fatigue cracks in the regime of up to approx- imately 10 7 cycles usually start from some kind of surface imperfections. Since that time, interior fatigue crack initiation has been discovered in other materials than high-strength steels as well. In addition, cracks were found to originate not only from inclusions, but also from interior pores or porous areas in cast aluminum alloys [4] or even from internal persistent slip bands in polycrystalline high purity copper [5] . Numerous investigations were performed to determine how structural features such as grain size, morphology and size of inclusions, surface treatment and pre-straining influence the fatigue strength and fatigue life of different materials such as

Corresponding author. Tel.: +43 1 47654 5160; fax: +43 1 47654 5159. E-mail addresses: ogawa@me.aoyama.ac.jp (T. Ogawa), stefanie.tschegg@boku.ac.at (S.E. Stanzl-Tschegg), bernd.schoenbauer@boku.ac.at (B.M. Schönbauer).

1 Tel.: +81 42 759 6203; fax: +81 42 759 6502.

2 Tel.: +43 1 47654 5169; fax: +43 1 47654 5159.

0013-7944/$ - see front matter 2013 Elsevier Ltd. All rights reserved.

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Nomenclature CT da /dN D f compact tension fatigue crack growth rate in m cumulative
Nomenclature
CT
da /dN
D f
compact tension
fatigue crack growth rate in m
cumulative damage
N
ODA
number of cycles
optically dark area within fish-eye fracture surface
R
SEM
S –N curve
D K
stress ratio
scanning electron microscope
plot of stress versus number of cycles to failure
stress intensity factor in MPa p m (defined by tensile component, i.e. amplitude of cyclic stress at R = 1 in
this paper)

Austenitic stainless steels [6] . A comprehensive overview of the most important findings by Li [7] was published recently. The study investigates the effects of hydrogen, vacuum, the boundary segregation of fine grains and carbides. According to Li, most of the fatigue life is spent on the formation of a characteristic fracture surface morphology. This characteristic fracture surface is called ODA (optically dark area) [8] because it looks dark when observed with an optical microscope, while the same region is also called FGA (fine granular area) [9] or GBF (granular bright facet) [10] based on the morphology. Thus, the terms correctly indicate the morphological characteristics and the term ODA is used in this paper, because optical microscopy was the main means of determining the sizes of the regions. Detailed fractography and transmission electron micrographs both led to corresponding roughness values of ODAs [9,11]:

compared to the original material microstructure, the grain size of the ODAs’ subsurface structure is extremely reduced [12] . Another remarkable characteristic of ODAs is that a similar morphology can be observed for different material systems, i.e. high strength steels [13] , titanium alloys [14–16] and aluminium alloys [17] . In addition, such a morphology can also be found on the fracture surface of compact tension (CT) specimens made of these materials for standard FCG tests when tested in a high vacuum environment [13,14,18,19]. Several theories try to explain the formation of ODAs: Murakami [20] emphasizes the influence of hydrogen, e.g. hydro- gen assisted fatigue crack growth. Oguma [12] proposes the segregation of extremely fine grains of material as influencing and accompanying ODA formation and Shiozawa et al. [21] emphasize the importance of the segregation of fine carbides and subsequent formation and coalescence of microcracks. At variable amplitude loading, beach marks were formed on the frac- ture surface of the fish-eye region around the ODA. These were used to characterize the ODA’s and fish-eye’s growth rate of an ODA using a fracture mechanics approach [22] . Only very few papers using fracture mechanical methods to quantify the areas of fish-eyes and especially ODAs around inclusions manage to give quantitative results for fatigue crack propagation rates and stress intensity factors [9,17,23–30] . In the present study, ultrasonic fatigue tests were performed on high carbon chromium bearing steel, SUJ2, and a precipitation hardened chromium–nickel–copper steel, 17-4PH, at constant amplitudes. Furthermore, two types of two-step amplitude stressing tests were conducted on SUJ2 steel in order to investigate the fatigue damage accumulation and the growth behav- ior of interior cracks. Based on these results together with those from the literature, a formation mechanism of the ODA is proposed.

2. Material and experimental procedures

The tested materials were SUJ2, a high carbon chromium steel for bearings (Japan industrial standards JIS) and 17-4PH, a precipitation hardened chromium–nickel–copper steel which is often used for steam turbine blades. Their chemical compo- sitions and mechanical properties are presented in Tables 1 and 2 , respectively. The SUJ2 steel was oil quenched from 850 C and tempered at 180 C for 120 min. The 17-4PH steel was age hardened at 620 C (condition H1150) and stress relief an- nealed at 600 C. The specimen shapes for the SUJ2 steel and the 17-4PH steel are shown in Fig. 1 (a) and (b), respectively. The surfaces of the test specimens were polished with abrasive paper in axial direction (final grade 2000 for SUJ2 and 4000 for 17-4PH).

Table 1 Chemical composition (mass%) of SUJ2 and 17-4PH steel.

Material

C

Si

Mn

P

S

Ni

Cr

Mo

Cu

Nb + Ta

O (ppm)

SUJ2

1.00

0.17

0.39

0.017

0.006

0.08

1.40

0.03

5.00

17-4PH

0.033

0.40

0.49

0.027

0.001

4.37

15.57

3.31

0.23

T. Ogawa et al. / Engineering Fracture Mechanics 115 (2014) 241–254

Table 2 Mechanical properties of SUJ2 and 17-4PH steel.

243

Material

Tensile strength (MPa)

Yield strength (MPa)

Young’s modulus (GPa)

Poisson’s ratio

Vickers’ hardness

Density (kg/m 3 )

SUJ2 a

205

0.28

747

7830

17-4PH b

1030

983

195

352

7800

a Quench: 850 C: 50 min., Temper: 180 C: 120 min.

b Condition H1150, Stress relieved at 600 C: 60 min.

b Condition H1150, Stress relieved at 600 C: 60 min. Fig. 1. Specimen shapes of SUJ2

Fig. 1. Specimen shapes of SUJ2 specimen (a) and 17-4 PH steel (b).

For the ultrasonic fatigue tests on the SUJ2 steel, a machine consisting of an ultrasonic welder (BRANSON Co., CR-20), a power supply (2000bcd) and software developed at Aoyama Gakuin University (where the experiments were performed) were used. The cyclic frequency of testing was 20 kHz, and the displacement amplitude at the specimen end lay between 10 and 50 l m. Fully reversed loading fatigue tests ( R = 1) were performed in laboratory air at 24 C with a relative humidity of less than 40%. The D r values were defined as the tensile component of the stress range for the experiments at R = 1 in this paper. In order to reduce specimen heating by the high-frequency ultrasonic vibration, compressed cold air was blown on the specimen surface using a vortex tube, the specimen temperature was monitored with a radiation thermometer and intermittent loading was employed: typical loading conditions in the constant amplitude test were 120 ms loading with 360–1500 ms pauses. The experiments on the 17-4PH steels were performed at the University of Natural Resources and Life Sciences in Vienna using closed-loop controlled ultrasonic equipment with vibration gauges serving as feed-back for the amplitudes [5,17]. The total strain ranges were, in addition, measured with small strain gauges (1 mm gauge length, 2.10 ± 1.0% gauge factor) resulting in a strain measurement accuracy of 2% in all cases. The stress ranges were determined from the strain ranges using Hooke’s law. Intermittent loading with pulse lengths of 2000–10000 cycles and pauses of 500– 1000 ms, depending on the amplitude, served to cool the specimens. The experiments were performed at R = 0.05 by super- imposing a static tension load with a servo-hydraulic machine. The test temperature was kept constant at 90 C. Besides constant amplitude loading, two-step and repeated two-step loading tests were performed on the SUJ2 steel. In the two-step tests (see Fig. 2 (a)), the initial stress amplitude D r 1 was 1200 MPa and was applied up to the average number of cycles to failure determined in the constant amplitude tests ( N 1 = 6.85 10 6 ). This was followed by a second stress ampli- tude, D r 2 with values between 1100 and 850 MPa, which was applied either until fracture occurred or until the shut-off number of cycles, N 1 = 1 10 10 , was reached (if no fracture occurred). In the repeated two-step tests, a higher stress amplitude D r H = 1200 MPa and lower stress amplitude D r L = 1050 or 850 MPa were repeated alternately until fracture, see Fig. 2 (b). Table 3 shows the different testing conditions used in the repeated two-step tests. Most of the tests began with the application of D r L followed by D r H , which is defined as one block. The number n H of cycles with D r H , was either n H = 1.0 10 3 or 1.0 10 4 , and the number n L of cycles with D r L was varied widely according to the n H / n L values indicated in Table 3 . The symbols used to designate the different testing conditions in the following figures are also listed in Table 3 . The cumulative damage, D f , is defined by Eq. (1) , where N Hf and N Lf are the numbers of cycles to failure for D r H and D r L , respectively, on the regression line of experimental data ( D r versus N F ) as shown in Fig. 3 . The cumulative damage for D r H is defined by Eq. (2) .

D f ¼ X

Hf þ X

N

n

H

n

L

N

Lf

ð 1Þ

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et al. / Engineering Fracture Mechanics 115 (2014) 241–254 Fig. 2. Schematic of two-step tests (a)

Fig. 2. Schematic of two-step tests (a) and repeated two-step tests (b).

Table 3 Testing parameters of four kinds of repeated two-step tests with symbols as used in Figs. 7, 9 and 10 .

D r L (MPa)

D r H (MPa)

Starting stress

n H (cycles)

n H / n L

Symbol

1050

1200

D r L

1.0 10 3 1.0 10 4 1.0 10 3

2.0 10 3 1.0 5.0 10 2 2.0 10 1 1.0 10 1 2.5 10 1 1.0 10 3 1.0

s

 

4

 

D r H

h

850

D r L

d

D H ¼ X Hf

N

n

H

3. Results and discussion

3.1. Constant amplitude and two-step amplitude tests

ð 2Þ

Fig. 3 displays the fatigue life diagram resulting from the constant amplitude and two-step amplitude tests on SUJ2. The line represents a linear regression of eight fatigue lives under constant amplitude loading. In the two-step amplitude tests,

constant amplitude loading. In the two-step amplitude tests, Fig. 3. S–N curve under constant and two-step

Fig. 3. S–N curve under constant and two-step loading of SUJ2 steel.

T. Ogawa et al. / Engineering Fracture Mechanics 115 (2014) 241–254

245

the first-step cyclic stress amplitude, D r 1 = 1200 MPa, was applied for N 1 = 6.85 10 6 , which corresponded to the average number of cycles to failure at this stress range in the constant amplitude tests. In order to avoid confusion, broken specimens under the first-step amplitude tests were ignored. Then a second-step cyclic stress amplitude was applied until all specimens which had survived the first step (in Fig. 3 , only those specimens are plotted) fractured. Therefore, the cumulative damage D f of these specimens exceeded unity. However, the N f values resulting from the secondary cyclic stress (added to the first step cyclic stress) were lower than the ones of the constant amplitude test, which suggests that the D f values lay below two. Fish-eye fractures originated from interior inclusions in all tested specimens. Fig. 4 shows the optical micrographs, depicting a specimen after the constant amplitude test at D r = 1200 MPa (a) and after the two-step test at D r 1 = 1200 MPa followed by D r 2 = 900 MPa (b). In both cases, ODAs, are visible, their sizes depending on the test conditions. An inclusion can be seen at the center of each ODA. The areas of the inclusion, ODAs and fish-eyes were measured and their square root values, p area , were used to calculate the stress intensity factor D K , using the equation for interior cracks [25] :

DK ¼ 0: 5 Dr

ffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi

q

p

p

ffiffiffiffiffiffiffiffiffiffi

area ;

ð 3Þ

D r being the stress amplitude for R = 1 or the stress range for R = 0.05. D K thus always corresponds to the tensile compo- nent of the cyclic stress. Fig. 5 (a) presents the square root of the inclusion sizes, p area Inc and their stress intensity value, D K Inc , as a function of D r for the SUJ2 and the 17-4PH steel: both p area Inc and D K Inc were independent of D r . The D K Inc values varied between 2.3 and 4 MPa p m. Fig. 5 (b) shows the square root value of the areas and the stress intensity factors for the ODAs, denoted as p area ODA and D K ODA , respectively. The values of D K ODA were almost constant, ranging from 5 to 5.5 MPa p m for both steels. This almost constant D K ODA value implies that this is the border line between the ODA and the fish-eye, i.e. a criterion for the transition of the crack from an ODA to the neighboring fish-eye area. Equally, the stress intensity values of D K FE for the fish- eyes in SUJ2 steel ( Fig. 6 ) were approximately constant, ranging from 16 to 21 MPa p m, which agrees with the fracture toughness measured in a standardized fracture mechanical test with a CT specimen. The asterisks in Fig. 6 mark the cases in which the fish-eyes joined the specimen surface. In these cases, D K FE was calculated using the following equation [25] :

DK ¼ 0: 65 Dr

ffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi

q

p

p

ffiffiffiffiffiffiffiffiffiffi

area

ð 4Þ

To summarize, the D K Inc and D K ODA values in the threshold regime were rather similar (assuming that only the tensile por- tion of cyclic loading contributed to the crack propagation) although two different steels were investigated: D K Inc lay be- tween 2.17 and 3.03 MPa p m and D K ODA was 5.02–5.79 MPa p m (cf. Fig. 5 ). These similarities were found even though different testing equipment was used and the R -ratio was different ( R = 1 for SUJ2 and R = 0.05 for 17-4PH).

different ( R = 1 for SUJ2 and R = 0.05 for 17-4PH). Fig. 4. Optical

Fig. 4. Optical micrographs of SUJ2 showing ODAs after a constant amplitude loading test at D r = 1200 MPa (a) and a two-step loading test at D r H = 1200 MPa followed by D r L = 900 MPa (b).

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et al. / Engineering Fracture Mechanics 115 (2014) 241–254 Fig. 5. Size and stress intensity factors

Fig. 5. Size and stress intensity factors of SUJ2 for cyclic stress amplitudes at fracture and cyclic stress ranges at fracture of 17-4PH steel for inclusions (a) and optically dark areas (b).

The run out specimen in Fig. 3 tested at D r 2 = 850 MPa (2nd step) was broken by subsequent fatigue loading at D r = 1200 MPa. On the fracture surface, a large ODA with D K ODA = 6.3 MPa p m was observed. This value is apparently larger than that of the D K ODA demonstrated in Fig. 5 (b) suggesting that the ODA grew due to the cyclic stress at D r = 850 MPa. In order to confirm this hypothesis, two similar experiments were conducted by applying different run-out numbers of cycles ( N = 2.0 10 9 and 3.0 10 10 ) at D r 2 = 850 MPa. In both tests, however, the specimens did not break at D r 2 = 850 MPa and were subsequently broken at D r = 1200 MPa. The calculated values of D K ODA for these two experiments were 5.3 and 5.1 MPa p m, respectively. These results indicate that in contrast to the above mentioned expectation, there is no growth of ODA at a cyclic stress of D r 2 = 850 MPa and that in addition, the statistical scatter of D K ODA values and the sizes of the ODAs is rather large.

T. Ogawa et al. / Engineering Fracture Mechanics 115 (2014) 241–254

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/ Engineering Fracture Mechanics 115 (2014) 241–254 247 Fig. 6. Sizes and stress intensity factors of

Fig. 6. Sizes and stress intensity factors of fish-eyes for stress amplitudes at fracture in SUJ2.

The resulting D K Inc and D K ODA values for different sizes of inclusions and ODAs in constant amplitude tests are summa- rized in Fig. 5 (a) and (b) for SUJ2 and 17-4PH steel. Although two different steels were investigated, their D K Inc and D K ODA in the threshold regime are rather similar – assuming that only the tensile portion of cyclic loading contributes to crack prop- agation -, with D K inc between 2.17 and 3.03 MPa p m and D K ODA 5.02–5.79 MPa p m, though different testing equipment was used and the R -ratio was different ( R = 1 for SUJ2 and 0.05 for 17-4PH).

3.2. Repeated two-step amplitude tests

Fig. 7 presents the cumulative damage at fracture D f , resulting from the repeated two-step amplitude tests, as a function of n H / n L . Furthermore, Fig. 7 also shows the value of the damage ratio by higher stress cycles, D H / D f , of the tests with D r L = 1050 MPa and 850 MPa. In the tests with D r L = 850 MPa (black dots), D H / D f was higher than 0.95 which indicates that D f was mainly caused by the higher stress cycles. When D r L was chosen to be 1050 MPa (open symbols), the scatter of the D f values was much larger, lying between 0.40 and 14.29, and no correlation with n H / n L was obvious. Since, however, in five of 33 experiments, D f values lower than one resulted, it is assumed that a two-step variation of the stress amplitude increases the fatigue life when increasing the ratio n L / n H .

fatigue life when increasing the ratio n L / n H . Fig. 7. Relationship between

Fig. 7. Relationship between cycle ratios and cumulative damage values (symbols explained in Table 3 ).

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A fish-eye fracture surface originating from an interior inclusion was observed in all he tested two-step specimens. Fig. 8 (a)–(c) show the optical micrographs of a specimen tested with the starting stress range of D r L = 850 MPa ( n L = 1.0 10 4 , n H = 1.0 10 3 and N f = 2.87 10 8 ) using different magnifications in order to show fish-eye, beach marks and ODA, respectively. ODAs can be seen around the inclusions in all the fractured specimens after two-step tests. Beach marks were identified in the fish-eye regions but not in the ODAs. The variation of the growth increment of the beach marks depended on the n H / n L values (see next section), and the relationships revealed that the dark and bright fracture surfaces corresponded to the crack growth increments caused by D r H and D r L , respectively. Fig. 8 (d) presents a scanning electron microscope (SEM) image of an ODA obtained by backscattering electron imaging; the morphology of the ODA region around the inclusion is granular. The stress variations were not visible in the high magnification SEM micrograph, which is in agree- ment with the optical result. The SEM observation indicated that the dark beach mark regions in the fish-eye region were slightly rougher than the bright one. The number of beach marks in the fish-eye region outside the ODA area indicated that the number of cycles to form this fracture surface was less than 1% of the total fatigue life, and most of the fatigue cycles were spent for the formation of the ODA. Therefore, the number of cycles to form an ODA is concluded to be approximately the same as the total fatigue life. Fig. 9 shows the relationship between p area Inc and n H / n L , where, as expected, no correlation could be found. This result and the mentioned tendency of D f to decrease with a decreasing ratio of n H / n L in Fig. 7 provides the relationship between D f and p area Inc shown in Fig. 10 . Ignoring the two exceptions of very small inclusion sizes, D f tended to decrease with an increasing p area Inc , and the values were smaller than the one for the three largest inclusions. This result implies that D f de- pends on the inclusion size at the fracture origin in the repeated two-step tests. Fig. 11 presents the variations of p area ODA and D K ODA with n H / n L . Some of the ODAs had different shades of darkness, as shown in Fig. 12 (a). As can be seen, the ODA is the darker interior region, and it is concluded that the widths of outer region represent different n H / n L conditions: this assumption is based on a comparison of the image with the SEM micrograph shown in Fig. 12 (b). The outer less dark region in Fig. 12 (a) grew due to a high stress range, similar to the beach mark region pre- sented in Fig. 8 (b). This fact suggests that the transition from ODA to fish-eye region occurred as soon as the high stress amplitude was applied, and thus D K ODA should be calculated for D r H = 1200 MPa. When n H / n L was larger than 0.1, the values of D K ODA were approximately the same as those presented in Fig. 5 (b) for constant amplitude and two-step tests. However, the ODAs tended to increase with decreasing n H / n L , i.e. increasing n L . This means that a high number of lower cyclic stresses augmented the size of the ODA. Such behavior can be explained by the following: when an ODA reaches the size at which its D K exceeds the constant value of D K ODA shown in Fig. 5 at D r H = 1200 MPa, a transition of the growth mechanism from the ODA to the fish-eye region mechanism may occur. If, due to the limited number of cycles, D K at D r L becomes lower than the critical D K ODA at the cyclic stress of D r L = 850 MPa, the growth mechanism returns to the ODA mechanism. This sequence is repeated until transition from ODA to fish-eye mechanisms occurs in the following way: when the high cyclic stress is

occurs in the following way: when the high cyclic stress is Fig. 8. Optical and scanning

Fig. 8. Optical and scanning electron micrographs showing a fish-eye (a), beach marks (b), an ODA (c) and an inclusion (d) for D r L = 850 MPa, n H = 1 10 3 and n L = 1 10 4 . Note that the red and blue arrows in (b) indicate the crack growth increment under high and low stress ranges, respectively.

T. Ogawa et al. / Engineering Fracture Mechanics 115 (2014) 241–254

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/ Engineering Fracture Mechanics 115 (2014) 241–254 249 Fig. 9. Relationship between cycle ratios and inclusion

Fig. 9. Relationship between cycle ratios and inclusion sizes under repeated two-step amplitude stressing (symbols explained in Table 3 ).

amplitude stressing (symbols explained in Table 3 ). Fig. 10. Relationship between inclusion sizes and

Fig. 10. Relationship between inclusion sizes and cumulative damage values D f under repeated two-step amplitude stressing (symbols explained in Table 3 ).

reapplied, D K becomes higher than D K ODA and the crack grows. When the stress is reduced, i.e. at the beginning of low cyclic stressing at a period of the high cyclic stress, where D K was higher than D K ODA, the crack ceases to grow. If the value of D K is calculated using the size of the outer contour of the dark area shown in Fig. 12 (a) together with D r L, a value of 8.8 MPa p m results, which exceeds the transition D K ODA by far. Oguma et al. [19] observed an ODA-like fracture sur- face morphology on fatigue fracture surfaces which had repeated contact in a high vacuum environment. This observation supports our theory of the ODA growth sequence: fish-eye growth increments change to ODA growth by the repeated surface contact under D r L conditions. This will be discussed in more detail in 3.4.

3.3. Growth characteristics of interior crack

The beach marks shown in Fig. 8 provide growth rates for the interior crack in the fish-eye region [22] . Fig. 13 represents the relationships of the crack growth rate, d a /d N , and the stress intensity factor range, D K .

d a /d N was

determined by D a L / n L or D a H / n H ; the corresponding D K was obtained from the area inside of the beach mark and the applied

D r according to Eq. (3). The error bars for D K in Fig. 13 correspond to the widths of beach marks, i.e. D a L or D a H . For com- parison, Fig. 13 also presents the growth characteristics of a long crack, which grew in a CT specimen in air at a stress ratio of 0.1 in a standard fracture mechanics test [31] : clearly, the interior crack growth rates obtained by the beach marks are lower than those observed on the CT specimen. A possible reason for this deviation is the environment: while it is assumed that interior cracks grow in a vacuum (the vacuum quality, however, has not been determined up to now), the crack in the CT specimen grew in air. To verify this assumption, crack growth experiments in vacuum are necessary, which, however, could not be performed with this material. Instead of that, fracture surfaces of crack propagation tests on 12% Cr steel in a vacuum of approx. 10 3 Pa

The crack growth increments for D r L and D r H are denoted D a L and D a H , respectively. The crack growth rate

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et al. / Engineering Fracture Mechanics 115 (2014) 241–254 Fig. 11. Sizes and stress intensity factors

Fig. 11. Sizes and stress intensity factors of ODAs under repeated two-step amplitude stressing.

factors of ODAs under repeated two-step amplitude stressing. Fig. 12. Micrographs showing a double shaded ODA

Fig. 12. Micrographs showing a double shaded ODA after tests with D r L = 850 MPa, n H = 1 10 3 and n L = 1 10 6 observed with an optical microscope (a) and a scanning electron microscope (b).

T. Ogawa et al. / Engineering Fracture Mechanics 115 (2014) 241–254

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/ Engineering Fracture Mechanics 115 (2014) 241–254 251 Fig. 13. Relationship between d a /d N

Fig. 13. Relationship between d a /d N and D K . Closed symbols: determined from measurements on CT specimens in air. Open symbols with D K in the range of 7 to 16 MPa: determined from measurements of fish-eye beach marks; open symbols with D K around 5 MPa: determined from radii of ODAs.

at 19 kHz and very high numbers of cycles are used and compared with the fracture morphology of ODAs [13] . It was con- cluded that within the ODAs, the growth rates were in the range of approximately 10 12 m/cycle. The growth rates in the ‘‘smooth’’ area adjacent to the ODAs were found to be below approximately 10 11 m/cycle [13] . Based on the similarities of the fracture morphologies of fish-eye regions and long-crack fracture surfaces formed in a vacuum, it was further con- cluded that fracturing occurs according to fracture mechanical laws for long cracks with rates depending on the prevailing stress intensity factor. As soon as the maximum stress intensity factor exceeds the threshold stress intensity factor for fati- gue crack propagation of long cracks, higher crack growth rates – ranging from around 10 9 m/cycle up to about 10 7 m/cy- cle – will occur outside the fish eye, thus forming the contour of the fish-eye. As stated earlier, the cycle ratio of this fish-eye growth phase to the total fatigue life is believed to be very small in comparison with the ODA growth and crack initiation stage. Concerning the environmental question, these studies confirm that vacuum is the crucial environment for fatigue crack propagation in the ODA, and the authors assume that it is justified to apply this result to the SUJ2 steel. Concerning fatigue crack growth within the whole fish-eye area (not only ODA), numerous interesting studies are re- ported in the literature. Since this paper, however, is focused on the ODA growth, only few important studies are mentioned. Petit and Sarrazin-Baudoux [31] developed a model based on plastic deformation accumulation controlling intrinsic crack propagation in vacuum. They estimated the life of high strength steels with cracks that initiated at a fish-eye and could show that the portion of life due to crack propagation in vacuum was two to three orders of magnitude greater than in air. This result confirms the measurements of this study. In [32] , ultra-slow fatigue crack propagation at ultrasonic frequency is treated. Murakami [20] discovered the influence of hydrogen content trapped around inclusions to play an important role during internal fatigue crack growth. The extremely low crack growth rates of the ODAs measured in the present study, however, rather exclude the influence of hydrogen. In a more recent study [33] , Murakami pointed out that ‘‘most of life cycles N f are spent in the ODA area’’. He distinguishes between material containing 0.8 ppm and, respectively, 0.1 ppm hydrogen (Cr–Mo steel SCM 435 after different heat treatment) and suggested a master curve for the number of cycles to failure N f versus ( p area ODA / p area Inclusion ). This curve showed material independence at a hydrogen content of 0.2–0.9 ppm. For material con- taining only 0.2–0.3 ppm hydrogen, a modified model for the fatigue limit was suggested considering that ‘‘the ODA grows as a crack’’. Further work is planned to apply this model to the results of the present study. The ODA growth rates in the two-step tests of the present study could be estimated making some assumptions, as ex- plained in the following: in the present study, the first step of D r 1 = 1200 MPa was applied up to a number of cycles that was somewhat smaller than the number of cycles to failure obtained in the constant amplitude test given in Fig. 3 . At this point, we assumed, an ODA of similar size as those observed in the constant amplitude tests at D r = 1200 MPa had been formed. In the subsequent second step, after applying a second defined stress D r 2 , this ODA then grew up to the size ob- served at fracture. In other words, we considered the ODA at D r 1 = 1200 MPa as a pre-crack, which grew at the cyclic stress amplitude during the second step without any effects of stress history. Fig. 13 shows the d a /d N values calculated by the ODA growth increment divided by the number of cycles to failure during the second step, in which the number of cycles to form a fish-eye was ignored owing to their much smaller values. The values of D K were determined by the D r of the second step together with the initial and final sizes of the ODA, whose corresponding values are characterized by the error bars. As can be seen, the growth rate of a fish-eye is ten to hundred thousand times larger than that of an ODA. This great difference in the growth rates seems to be the most probable reason for the apparent change in the fracture surface morphology.

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3.4. Mechanism of ODA formation

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For further investigation of the mechanism of ODA formation, three-dimensional fracture surface observations were per- formed using an atomic force microscope (AFM, Keyence Co. VN-8000) for two different conditions of repeated two-step tests, i.e. n H / n L = 0.20 and 0.02 for n H = 1.0 10 3 . Fig. 14 presents surface roughness profiles resulting from these two differ- ent testing conditions: AFM1 and AFM2 are images of the two opposite fracture surfaces of a specimen after testing with n H / n L = 0.20 (a) and n H / n L = 0.02 (b). The graphs on the right show the sectional appearances along the dashed lines in the photos on the left, which are considered to be corresponding locations. The sectional appearances revealed that the pair of the ODA surfaces match nicely, as reported earlier by Shiozawa et al. [9,21]. In the past, significant suggestions for the mechanism of ODA formation were made. Some came from Oguma et al. [12] as mentioned above, from Furuya et al. [27,28] and Nakajima et al. [29] , who studied the development of ODAs, crack initiation and fatigue limit of SUJ2 steel with two-step loading tests with a rotating bending machine. Other important inputs came from Murakami et al. [20], Murakami and Matsunaga [33] and Petit and Sarrazin [31,32] as mentioned above. The present study revealed that the growth of ODAs is ten to hundred thousand times slower than that in the outer fish- eye regions, though both may be assumed to occur in a vacuum. Also, in the repeated two-step tests, the growth increment under high stress amplitudes obviously changed to ODA growth, as was concluded from the experiments with higher run- out numbers of cycles at the ‘‘high’’stress amplitudes (cf. last paragraph of 3.1). This was probably due to the repeated con- tact under the low stress amplitude. Higher growth rates after the beginning of ODA formation owing to the initial absence of crack closure effects could not be observed in this study, but cannot be excluded. The very slow growth of the ODAs may be explained by the following mechanism based on Oguma’s study [19] , which applies to ODA formation: it is assumed that the ODA morphology is formed by repeated fracture surface contact. In a vac- uum, fracture surface roughness induces local contact, so that such locations may re-bond (cold-weld) because the surface is active in a vacuum. During the following loading, the welded location may undergo plastic deformation and local cold work may occur. These considerations are based on numerous pioneer studies on fatigue crack initiation and propagation being influenced by contact of rough fracture surfaces, rewelding of fresh fracture surfaces and enhanced plasticity thus leading to longer fatigue lifes [34–37]. If fatigue loading is repeated for a long time, the local cold work may produce fine grains as observed by Oguma et al. [12] in the TEM. The results strongly suggest that the repeated contact in a vacuum produces the ODA morphology. Since ODAs grow extremely slowly and discontinuously, the repeated fracture surface contact in a vac- uum takes place very often, so that a very fine grained microstructure is formed. Thus, the darkness of the ODA seems now to have the consensus interpretation of being caused by an extreme surface roughness associated with a fine granularity. Fur- ther investigations, for example, introducing Murakami’s ideas [33] are needed to clarify the mechanisms being relevant for the ODA formation. The diffusive nature of the process of small grain formation could be explained as follows: low stress amplitudes, as those discussed above, lead to shear crack propagation, which produces multiple crack plane deviations. Thus, the local strains at the asperity interactions and the crack tip are probably very high and would therefore induce very intense point defect cre- ation. This is one possible cause of a diffusive transformation in the near crack surface grain structure. Another possible cause can be excluded, namely a significant global temperature rise in the specimen owing to the high frequency of stressing. Such a global heating was refuted by comprehensive experimental measurements [5] . Very localized temperature increases, how- ever, cannot be excluded, so that both welding and recrystallization would be possible. An important argument against a

would be possible. An important argument against a Fig. 14. Surface roughness profile of a fracture

Fig. 14. Surface roughness profile of a fracture surface after repeated two-step amplitude stressing; D r L = 1050 MPa, n H = 1 10 3 and n L = 5 10 3 (a), D r L = 1050 MPa, n H = 1 10 3 and n L = 5 10 4 (b).

T. Ogawa et al. / Engineering Fracture Mechanics 115 (2014) 241–254

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/ Engineering Fracture Mechanics 115 (2014) 241–254 253 Fig. 15. SEM images of ODAs in AISI

Fig. 15. SEM images of ODAs in AISI 420 Cr-steel (a), in AISI 316L-PM/HP steel (b) and spray formed hypereutectic Al-Si alloy (c).

high-frequency influence is offered by the results of Furuya et al. [27] . They found ODAs at testing frequencies of 100 Hz, 600 Hz and 20 kHz around inclusions of Al 2 O 3 or Al 2 O 3 .CaO and, in addition, a frequency independence of the S N diagrams for low-temperature-tempered JIS SNCM430 steel. As can be concluded from the above mentioned considerations, ODAs are probably formed by repeated fracture surface contact in a vacuum without the influence of the original material microstruc- ture such as grain size. This interpretation also implies that ODA formation is a crack propagation mechanism and cannot be considered as crack initiation, as assumed by a few authors (e.g. [30] ). After hydrogen and fine carbides were found to affect the growth rates of ODAs [12,20,21]. the finding of the present study that the ODAs’ morphology was independent of these influences seems interesting. The other characteristic of ODAs – their presence in different materials (in high-strength steels [7,9–12,22,27–29] , titanium alloys [15,16,18,19] , medium strength alloy steel [13,38,39] and Al alloys [17] ) – is corroborated by examples of ODAs in AISI 420 Cr steel, AISI 316L-PM/HIP steel and spray formed hypereutectic Al–Si alloy in Fig. 15 .

4. Conclusion

In the present study, ultrasonic fatigue tests at constant amplitudes were carried out on SUJ2, a high-strength carbon chromium bearing steel, and 17-4PH, a precipitation hardened chromium-nickel-copper steel at constant amplitudes. In addition, two-step and repeated two-step amplitude tests were performed on the SUJ2 steel in order to investigate fatigue damage accumulation and growth behavior of interior cracks. The results obtained are summarized in the following:

(1). In all steels tested in the present study, the fracture origin was from an interior inclusion, around which an optically dark area (ODA) and fish-eye regions were observed. Their sizes decrease with increasing stress amplitude, whereby the stress intensity factors (SIF) remain approximately constant. (2). In the repeated two-step amplitude stress tests, the cumulative damage D f scattered between 0.40 and 14.29. Five of 33 cases of testing conditions resulted in a D f value below unity. It was thus concluded that variations of the stress amplitude increase the fatigue life. The D f values decrease with increasing inclusion size, while their dependence on the cycle ratio of high and low stress amplitudes remained unclear. (3). Fatigue crack growth characteristics expressed by the relationships between the growth rate d a /d N and the stress intensity factor range D K were determined by beach marks in the fish-eye region which resulted from the repeated two-step tests and the differences in ODA sizes which resulted from the two-step tests. The growth rates of the fish-eyes were smaller than those for long cracks obtained by fracture mechanics experiments in air, and ten or hun- dred thousand times higher than those of the ODAs. (4). It is estimated that the ODA morphology is formed by repeated fracture surface contact in a vacuum, i.e. in the interior of material, and is not determined by its growing mechanism which, however, causes a disintegration the original microstructural features.

Acknowledgements

The present research was conducted as a cooperative work of GCF3 committee of The Japan Welding Engineering Society supported by Kyusyu Electric Power Co., Inc., Hokkaido Electric Power Co. Inc., Tohoku Electric Power Co. Inc., Tokyo Electric Power Company, Chubu Electric Power Co., Inc., Hokuriku Electric Power Company, The Kansai Electric Power Co., Inc., The Chugoku Electric Power Co., Inc., Shikoku Electric Power Co. Inc., The Japan Atomic Power Company and Electric Power Development Co., Ltd. The SUJ2 specimens were provided by Yukio Matsubara of NTN Corporation. The experiments on the 17-4PH steel were performed within a research project of the Electric Power Research Institute (EPRI), USA, and the Uni- versity of Natural Resources and Life Sciences, Austria. Language support by Dipl.-Ing Veronika Doblhoff-Dier is gratefully acknowledged. We also thank two of the reviewers for their constructive criticism, which we implemented in Sections 3.3 and 3.4.

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