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www.sciencemag.org/content/355/6329/1055/suppl/DC1
Supplementary Materials for
Bone-like crack resistance in hierarchical metastable nanolaminate steels
Motomichi Koyama,* Zhao Zhang, Meimei Wang,* Dirk Ponge, Dierk Raabe, Kaneaki Tsuzaki, Hiroshi Noguchi, Cemal Cem Tasan*
*Corresponding author. Email: [email protected] (M.K.); [email protected] (M.W.);
[email protected] (C.C.T.)
Published 10 March 2017, Science 355, 1055 (2017) DOI: 10.1126/science.aal2766
This PDF file includes:
Materials and Methods Supplementary Text Figs. S1 to S8 Tables S1 and S2 References
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Materials and Methods
Materials
The ferrite-martensite Fe–0.9C–1.7Mn–0.24Si (wt.%) dual phase (DP) steel (Fig. 1C)
was produced by intercritical annealing at 1023 K and follow-up quenching to room
temperature. The ferrite-cementite Fe–0.9C–0.9Mn–0.4Si (wt.%) pearlitic steel (Fig. 1D)
was heat treated at 1200 °C for 30 min, followed by 650 °C for 3 min, and quenched in
water. The pearlite block size and lamellar spacing were approximately 75 μm and 0.15
μm, respectively. The metastable multiphase martensite-austenite TRIP steel (Fig. 1E) had
a chemical composition of Fe-9Mn-3Ni-1.4Al-0.01C (wt. %). The steel was cast and hot
rolled at 1373 K. Afterwards, it was homogenized at 1373 K for 1 hour and subsequently
water-quenched. The as-quenched steel plate was cold rolled by 70% thickness reduction.
Partial reversion of cold-rolled αʹ-martensite to austenite was carried out at 873 K for 1 h
(37: M.-M. Wang, C.C. Tasan, D. Ponge, D. Raabe, Spectral TRIP enables 1.1 GPa
martensite. Acta Materialia 111, 262-272 (2016).). The new metastable multiphase
nanolaminate steel (Fig. 1F) introduced in this study has a Fe-9Mn-3Ni-1.4Al-0.01C
(wt.%) composition. The steel was cast and hot rolled at 1373 K. Afterwards, it was
homogenized at 1373 K for 1 hour and subsequently water-quenched. The as-quenched
microstructure was fully lath martensitic. For obtaining reversed austenite with different
volume fractions, the as-quenched martensite bulk specimens were annealed at 873 K for
1 and for 8 hours, respectively (17, 18). This treatment produced a martensitic matrix with
austenite islands at various martensitic boundaries. The latter can be classified into two
groups based on their size: those that range between 0.1 - 0.3 μm2 and the others that are
between 0.3 - 4.0 μm2. As reference material in Fig. 2 we use a DP steel with coarse and
equiaxed grain shape. Specific martensite or ferrite morphologies such as laminated α/α’
that can deflect the fatigue crack path provide similar fatigue crack resistance to pearlitic
steels. Other mechanical tests of the metastable multiphase nanolaminate steels reveal
improvements in fracture toughness as well as in tensile elongation (18).
Methods
Fatigue properties were evaluated by rotary bending fatigue testing at 50 Hz at room
temperature (≈ 298 K). The stress ratio, R, was −1, and a sinusoidal waveform was
employed. The stress ratio is defined as the minimum stress divided by the maximum
stress. To reduce the effect of temperature increase during testing, the specimens were
cooled by an electric fan. The fatigue cracks were observed by optical microscopy using
the replica technique (38: S. Hamada et al., Strain mapping with high spatial resolution
across a wide observation range by digital image correlation on plastic replicas. Materials
Characterization 98, 140-146 (2014).). Prior to testing, the specimens were mechanically
polished with emery papers and colloidal silica. The polished specimens were chemically
etched with 3% nital to reveal the microstructures. In terms of instrumentation, we used an
Ono-type rotary bending fatigue test machine (specimens were clamped on both sides.)
(39: M. Ohnami, Fracture and society, IOS Press, 180 (1992).). The specimen geometry is
given in Fig. S1. After fatigue testing, sample surface was prepared following standard
metallography procedures. Samples were prepared by grinding, polishing in diamond
suspension and final polishing in colloidal silica suspension. The last step ensures obtaining
a deformation-free surface.
In addition, to clarify the high importance of the nanolaminate microstructure
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morphology for the improved properties, we carried out corresponding fatigue tests also
for the same material, yet, with non-laminated metastable multiphase microstructure
presented in Fig. 1E. Since the design of the non-laminated metastable multiphase
microstructure requires cold rolling, the resulting specimen geometry is always a plate.
Therefore, the fatigue test plate specimen was fixed on the round bar jig as shown in Fig.
S3, and fatigue tests were performed on an Ono-type rotating bending fatigue testing
machine at room temperature with a stress ratio of −1 and a frequency of 30 Hz. Results of
this additional experiments are presented in Fig. S4. All of the results presented in Fig. S4
were obtained from the same plate specimen geometry and testing method.
Microstructures were characterized by scanning electron microscopy based EBSD at
15 kV at a beam step size of 80 nm and ECCI at 20 kV. Samples for the SEM analyses
were prepared by grinding, polishing in diamond suspension and final polishing in colloidal
silica suspension.
Supplementary Text
Fatigue crack closure
In this study, we observed crack termination associated with roughness of the crack
surface and metastability of austenite. The termination mechanisms of fatigue cracks
observed here have been understood as crack closure effects, which is different from the
crack arrest mechanisms observed in fracture toughness testing. Since fatigue cracks are
re-sharpened by compression, fatigue crack growth cannot be terminated by crack blunting
which typically reduces stress concentration at a crack tip. Instead, cyclic loading produces
compressive residual stresses on a crack surface, suppressing plastic deformation at a crack
tip during crack opening. This mechanism is typically referred to as plasticity-induced
crack closure. Volume expansion by αʹ-martensitic transformation enhances this crack
closure effect, a mechanism which is then referred to as transformation-induced crack
closure (25, 28, 29). Crack surface roughness also contributes to the enhancement of the
crack closure properties through strengthening effects contributed by compressive residual
stresses and friction stresses acting on the crack surface (24, 27). Specifically, fatigue
cracks are terminated when the following conditions are satisfied.
1) Dislocation emission at a fatigue crack tip does not occur. 2) Brittle cracking does not occur Even when a fatigue crack is not terminated, the fatigue crack growth is decelerated by
the crack closure effects, improving fatigue life.
Difference between rotary bending fatigue and pull-push fatigue tests
There is a difference between the rotary bending fatigue test and the pull-push fatigue
test due to the presence of stress gradients (40: D.C.R. Waryoba, J.S. Mshana, Effect of
size and stress gradient on fatigue behavior. International Journal of Pressure and Piping
60, 177-182 (1994).). Yet, this effect does not change the order and trend of fatigue life
and fatigue limit values obtained on specimens without notch in the comparison shown in
Fig. 2. Stress gradients lead to slightly higher fatigue strength values in rotary bending
fatigue tests (Fig. S5). Here, we consider effects of stress gradients on fatigue limit and
fatigue life separately. The fatigue limits presented in this study are determined by fatigue
crack initiation and non-propagation limits. The length of a non-propagating crack that
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must be considered for fatigue limit is less than 140 μm as demonstrated in Fig. 3d.
Assuming a half-penny shaped crack, the depth of the small crack is 70 μm when counted
from the specimen surface. This means that a reduction in stress pertaining to the stress
gradient is negligibly small in the current case, which does not affect the small crack
behavior. Also for fatigue life, the major portion of the life span is composed of (a) the
fatigue crack initiation life span and (b) the small fatigue crack propagation life span. In
fact, 80% of the total fatigue life value is dominated by fatigue crack growth until 1 mm as
shown in Fig. S6. More specifically, for the case of fatigue life, the depth of the crack is
around 500 μm, which is still a small effect on stress reduction. The reminder of the 20%
of the fatigue life span may be influenced by the effect of stress gradients, which means
that the fatigue life span presented in this study may be overrated slightly. However, all the
other reference data used in this study were taken by the same experimental method and
on specimens with similar geometry. Therefore, the difference between rotary bending
fatigue testing and push-pull testing similarly affects respective experimental results of the
resent alloys and reference materials.
Comparison of the current findings with the properties of other conventional structural
materials
The data sets shown in Fig. S7 provide a wider comparison range in fatigue properties
of our new hierarchical nanolaminate steel with other structural materials including type
304 austenitic steel and Ti-based alloys. Even compared to the austenitic steels and Ti-
based alloys, the fatigue life values of the present metastable multiphase nanolaminate
steels are concluded to be superior particularly at high stress amplitudes.
Crack surface roughness and its effect on crack motion
Fig. S8 shows a SEM image showing a sub-crack with a distinct roughness in the
metastable multiphase nanolaminate steel. As indicated by the yellow arrows, some parts
of the crack surfaces contact each other, while other portions do not. The mismatch between
the crack surfaces during crack opening and closing processes prevents fatigue crack
growth, a mechanism which has been referred to as roughness-induced crack closure (25).
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Fig. S1
A schematic sketch of the specimen geometry used for the rotary bending fatigue tests.
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Fig. S2
Replica images showing fatigue crack initiation at a non-metallic inclusion of the presented
steel aged for 1 h tested at 500 MPa. (A) Before and (B) after testing until 2×105 cycles.
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(A)
(B)
Fig. S3
(A) A schematic sketch of the plate specimen geometry used for the fatigue tests (unit:
mm). A jig shown in (B) was used to test samples taken from the plate specimens by
rotating bending fatigue testing. The plate specimen was fastened on the jig by screws.
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Fig. S4
Stress amplitude vs. number of cycles to failure diagram of the presented steel in a
microstructural state once with and once without a nanolaminate microstructure.
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Fig. S5
Comparison between fatigue strength values measured by rotary bending fatigue testing
and by pull-push fatigue testing (41: T. Araki, NRIM Fatigue Data Sheet No. 2, (National
Research Institute for Metals, 1978). 42: T. Araki, NRIM Fatigue Data Sheet No. 3,
(National Research Institute for Metals, 1978). 43: T. Araki, NRIM Fatigue Data Sheet No.
4, (National Research Institute for Metals, 1978). 44: S. Nishijima, Fundamental fatigue
properties of JIS steels for machine structural use, NRIM fatigue data sheet technical
document No. 5, (National Research Institute for Metals, 1981).). The chemical
compositions of these steels are listed in Table S1.
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Fig. S6
Fatigue crack length plotted against number of cycles at 760 MPa observed in the new
metastable nanolaminate steel aged for 1 h.
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Fig. S7
Comparisons of fatigue life values determined for various materials including type 304
austenitic steel (45: N. Hattori, S. Nishida, A. Takahashi, Effect of structure stability on
fatigue properties of austenite stainless steels. Transaction of the Japan Society of
Mechanical Engineering Series A 65, 340-344 (1999).) and Ti-based alloys (46: L.
Wagner, Mechanical surface treatments on titanium, aluminum and magnesium alloys.
Materials Science and Engineering A 263, 210-216 (1999)). Some of data obtained for the
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Ti-based alloys and for the type 304 steel were tested with the same method as the samples
of the new metastable multiphase nanolaminate steels in our laboratory. The chemical
compositions of the steels tested in our laboratory are listed in Table 2.
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Fig. S8
SEM image showing roughness and associated crack surface contact of the presented steel
aged for 1 h tested at 800 MPa. The yellow arrows specifically indicate parts of the crack
surface contacting each other. The specimen surface was mechanically polished up to depth
of 48 μm and subsequently etched by 3% nital after the fatigue test. This crack is one of
the sub-cracks that exist after the failure.
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Table S1.
Chemical compositions (wt. %) of the steels used for Fig. S5 (41: T. Araki, NRIM Fatigue
Data Sheet No. 2, (National Research Institute for Metals, 1978). 42: T. Araki, NRIM
Fatigue Data Sheet No. 3, (National Research Institute for Metals, 1978). 43: T. Araki,
NRIM Fatigue Data Sheet No. 4, (National Research Institute for Metals, 1978). 44: S.
Nishijima, Fundamental fatigue properties of JIS steels for machine structural use, NRIM
fatigue data sheet technical document No. 5, (National Research Institute for Metals,
1981).). The steels marked by yellow and gray were used for determining fatigue strength
data at 105 and 2×107 cycles, respectively. -: Not examined
C Si Mn P S Ni Cr Mo Cu
S35C
A 0.35 0.21 0.77 0.021 0.022 0.01 0.01 - 0.02
B 0.35 0.30 0.74 0.017 0.024 0.01 0.10 - 0.01
C 0.34 0.26 0.74 0.012 0.015 0.01 0.02 - 0.01
D 0.36 0.26 0.70 0.009 0.023 0.08 0.12 - 0.09
S45C
A 0.45 0.25 0.79 0.018 0.016 0.02 0.13 - 0.02
B 0.45 0.26 0.76 0.027 0.019 0.01 0.11 - 0.02
C 0.45 0.24 0.71 0.010 0.009 0.12 0.06 - 0.13
D 0.44 0.24 0.82 0.021 0.021 0.03 0.02 - 0.03
S55C
A 0.55 0.23 0.76 0.018 0.012 0.01 0.09 - 0.01
B 0.54 0.26 0.76 0.022 0.021 0.02 0.12 - 0.01
C 0.52 0.29 0.83 0.016 0.025 0.04 0.04 - 0.02
D 0.56 0.26 0.67 0.019 0.026 0.04 0.13 - 0.11
S35C Max 0.38 0.30 0.82 0.031 0.030 0.08 0.12 - 0.11
Min 0.32 0.21 0.63 0.007 0.013 Ni + Cr = 0.02~0.20 - 0.01
S45C Max 0.49 0.26 0.83 0.027 0.025 0.13 0.13 - 0.15
Min 0.42 0.22 0.70 0.010 0.009 Ni + Cr = 0.03~0.18 - 0.01
S55C Max 0.57 0.30 0.83 0.024 0.026 0.06 0.13 - 0.22
Min 0.52 0.20 0.67 0.009 0.012 Ni + Cr = 0.02~0.17 - 0.01
SMn438 Max 0.46 0.27 1.59 0.017 0.019 0.06 0.22 - 0.08
Min 0.38 0.21 1.34 0.011 0.007 0.02 0.03 - 0.02
SMn443 Max 0.46 0.34 1.60 0.027 0.022 0.10 0.27 - 0.10
Min 0.40 0.21 1.36 0.008 0.007 0.02 0.04 - 0.01
SCr440 Max 0.43 0.32 0.81 0.022 0.014 0.07 1.12 - 0.13
Min 0.39 0.22 0.71 0.010 0.004 0.02 0.94 - 0.01
SCM435 Max 0.38 0.35 0.82 0.026 0.022 0.12 1.09 0.19 0.19
Min 0.33 0.23 0.69 0.012 0.007 0.01 0.97 0.15 0.01
SCM440 Max 0.44 0.29 0.87 0.024 0.028 0.24 1.10 0.22 0.15
Min 0.37 0.22 0.69 0.010 0.004 0.02 0.94 0.15 0.02
SNC631 Max 0.35 0.30 0.65 0.019 0.016 2.78 0.89 - 0.10
Min 0.28 0.22 0.49 0.008 0.004 2.63 0.71 - 0.05
SNCM439 Max 0.43 0.33 0.79 0.022 0.021 1.92 0.96 0.24 0.12
Min 0.37 0.19 0.68 0.010 0.004 1.62 0.68 0.16 0.03
SNCM447 Max 0.49 0.29 0.79 0.014 0.016 1.80 0.79 0.20 0.11
Min 0.44 0.16 0.69 0.009 0.009 1.65 0.71 0.16 0.05
SUS403 Max 0.15 0.50 0.83 0.029 0.023 0.31 12.70 0.15 -
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Min 0.09 0.21 0.32 0.016 0.002 0.08 11.65 0.02 -
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Table S2.
Chemical compositions of the reference materials for Fig. S7. -: Not examined.
Fe C Mn P S Ni Cr Ti Al N O V
Type 304
austenitic
steel
Bal. 0.046 0.84 0.02 0.005 8.7 18.42 0.002 0.001 0.044 - -
Ti-based
alloy 0.225 - - - - - - Bal. 6.29 - 0.155 4.35
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aal2766-Koyama-SM.ref-list.pdfReferences and Notes