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Materials Science & Engineering A 666 (2016) 1926

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Materials Science & Engineering A


journal homepage: www.elsevier.com/locate/msea

Defect-dominated fatigue behavior in type 630 stainless steel


fabricated by selective laser melting
Masayuki Akita a,n, Yoshihiko Uematsu b, Toshifumi Kakiuchi b, Masaki Nakajima c,
Ryosei Kawaguchi d
a
Faculty of Engineering, Gifu University, 1-1 Yanagido, Gifu 501-1193, Japan
b
Department of Mechanical Engineering, Gifu University, Yanagido, Gifu 501-1193, Japan
c
National Institute of Technology, Toyota College, 2-1 Eisei-cho, Toyota 471-8525, Japan
d
Mechanical and Systems Engineering Division, Graduate School of Engineering, Gifu University, 1-1 Yanagido, Gifu 501-1193, Japan

art ic l e i nf o a b s t r a c t

Article history: Fatigue behavior of type 630 (174 pH) stainless steel specimens fabricated by selective laser melting
Received 1 March 2016 (SLM) was studied. The results obtained were compared with those of the conventionally-melted (CM)
Received in revised form type 630. In the microstructure of SLM type 630, martensite-poor and ferrite-rich areas were recognized,
12 April 2016
while in the CM type 630, acicular martensite uniformly distributed in a matrix. Relatively high tem-
Accepted 13 April 2016
Available online 14 April 2016
perature was held due to the additive lamination of melted powder during SLM process, which pre-
vented full-martensite structure formation. In the SLM-quenched type 630, the microstructure consisted
Keywords: of acicular martensite due to the post heat treatment at 1050 C followed by water quenching. The
Fatigue hardness was the highest in the CM type 630, and followed by SLM-quenched and SLM type 630 in
Selective laser melting
decreasing order. The microstructural observation revealed that some defects ( o 50 mm) distributed in
Martensitic stainless steel
the SLM and SLM-quenched type 630, which were formed during additive lamination of melted powder.
Microstructure
Crack initiation Rotating bending fatigue tests were performed at a frequency of 57 Hz in laboratory air. The SLM and
Crack growth SLM-quenched type 630 exhibited much lower fatigue strengths compared to the CM one. One of the
reasons of lower fatigue strengths in the SLM and SLM-quenched type 630 could be attributed to their
lower hardness. Furthermore, fatigue cracks initiated from the defects in both SLM type 630. Conse-
quently, fatigue crack initiated at an early stage of fatigue life in the SLM and SLM-quenched type 630,
resulting in the lower fatigue strengths. However, fatigue crack growth resistances of the SLM and SLM-
quenched type 630 were higher than that of the CM one due to frequent crack branching and deection.
& 2016 Elsevier B.V. All rights reserved.

1. Introduction workability, namely maraging steels, titanium alloys and pre-


cipitation-hardening stainless steels, and etc.
Selective laser melting (SLM) method is one of the additive Type 630 (174 pH) stainless steel is one of the precipitation-
manufacturing (AM) processes, in which metallic powder is se- hardening martensitic stainless steels and is widely used in var-
lectively melted and fused by a high energy density laser beam [1 ious industry elds due to high strength, good ductility and ex-
3]. This fabricating method allows the production of machine cellent SCC resistance [1012]. On the other hand, type 630 has
components using an information from a three-dimensional poor workability caused by high strength. It takes much time and
model CAD data [4]. Compared with conventional manufacturing cost to obtain desired shape of product when using conventional
methods, SLM offers distinct advantages in terms of design free- fabricating methods. Therefore, the fabrication by SLM method for
dom, free of tooling, near-net or net shape production, efcient the functional products with a complex geometry is so effective
[13].
use of materials, short lead time and cost savings without dies or
The microstructure of material fabricated by SLM method is
substantial machining [3,5,6]. Therefore, SLM technology is greatly
different as compared to conventionally-processed material. In
applicable for the use in high value applications such as aerospace
addition, many machine components are subjected to cyclic stress.
and biomedical industries [79]. In addition, this technology is
Therefore, it is important to clarify the fatigue properties of ma-
particularly applied to the materials with high strength and poor terials fabricated by SLM method. Though the fatigue properties of
titanium alloys and type 316 L stainless steels processed by SLM
n
Corresponding author. method have been described in several studies [1418], the studies
E-mail address: akita@gifu-u.ac.jp (M. Akita). on the fatigue properties including crack growth behavior of type

http://dx.doi.org/10.1016/j.msea.2016.04.042
0921-5093/& 2016 Elsevier B.V. All rights reserved.
20 M. Akita et al. / Materials Science & Engineering A 666 (2016) 1926

630 stainless steel made by SLM method are very limited [18].
In the present study, rotating bending fatigue tests were con-
ducted using type 630 stainless steel fabricated by SLM method.
Based on the results obtained, the fatigue behavior and fracture
mechanism in the material made by SLM method were discussed
through the comparison to the results of conventional type 630.

2. Materials and experimental procedures


Fig. 1. Conguration of fatigue specimen.

2.1. Materials preparation


Table 1
Mechanical properties of type 630.
In the present study, pre-alloyed type 630 stainless steel
powder was used for the SLM by the additive manufacturing in an Specimen Proof Tensile Elongation Reduction Elastic
EOSINT M280 system. This SLM machine uses Ytterbium-ber la- stress strength (%) of area (%) Modulus E
ser. The processing parameters used were as follows; the max- s0.2 sB (MPa) (GPa)
imum laser output power, the focus diameter and lamination laser (MPa)

thickness were 400 W, 0.1 mm  0.5 mm, 0.02 mm 0.05 mm, CM specimen 1011 1089 9 68 174
respectively. The other detailed SLM process parameters are not
disclosed from a material supplier. It is well known that the me-
chanical properties of SLM-fabricated materials depend on the 600
build direction [1926]. In the present study, lamination plane was
parallel to the longitudinal direction of the specimen. These spe-
cimens were referred as SLM specimen. It is considered that the
cooling rate of additively layered powder is slow, because melted 500
power is continuously supplied on the lamination plane. There- Vickers hardness HV
fore, a post heat treatment was given to the SLM specimen, in
which the temperature was held at 1050 C for 4 h, followed by 400
water quenching. This material was designated as SLM-quenched
specimen. Furthermore, the conventional type 630 stainless steel
was also prepared. The chemical composition (wt%) of the con-
ventional type 630 was as follows; Cr: 15.58, Ni: 4.22, Cu: 3.31,
300
Mn: 0.81, P: 0.35, Nb: 0.28, Si: 0.26, C: 0.04, S: 0.01, Fe: bal. This
material had been solution treated at 1050 C for 1 h, followed by
water quenching in the as-received condition. Hereafter, this ma- 200
terial was referred as conventionally melted (CM) specimen.
The smooth round-bar fatigue specimens with a diameter of
8 mm and a gauge length of 10 mm were fabricated by the SLM
100
method as shown in Fig. 1. Prior to fatigue tests, the gauge section
SLM SLM CM
of specimen was mechanically polished using progressively ner quenched
grades of emery paper followed by buff-nish. Table 1 shows the
mechanical properties of CM type 630 after solution treatment. In Fig.2. Vickers hardness.
the SLM and SLM-quenched specimens, tensile test was not per-
formed due to the limitation of sample number. hardness was 275 HV, 340 HV and 454 HV for the SLM, SLM-
quenched and CM specimens, respectively. Hardness in the CM
2.2. Experimental procedures specimen was the highest and followed by the SLM-quenched and
SLM specimens in decreasing order.
Fatigue tests in laboratory air at an ambient temperature were The 3D appearance of microstructure in the SLM specimen is
performed using an Ono-type four-point rotating bending fatigue shown in Fig. 3(a). The anisotropy depending on the build direc-
testing machine with a capacity of 98 Nm operating at a frequency tion was not identied in the microstructure. Fig. 3(be) show the
of 57 Hz. The crack initiation and early crack growth were mon- SEM micrographs of microstructures in the SLM and SLM-quen-
itored by a plastic replication technique. After fatigue tests, frac- ched specimens. In the SLM specimen (Fig. 3(b and c)), ferrite-rich,
ture surfaces were examined in detail using a scanning electron namely martensite-poor areas are recognized as shown by the
microscope (SEM). The microstructures of three types of speci- arrows in the gure. On the other hand, the microstructures of the
mens were also observed using an SEM. Measurements of hard- SLM-quenched specimen (Fig. 3(d and e)) are more uniform, and
ness were carried out using a Vickers micro-hardness tester (test consist of rough acicular martensite. It is due to the transformation
load: 4.9 N, load-holding time: 30 s). from austenite to martensite by water quenching. The micro-
structures of the CM specimen are shown in Fig. 3(f) and (g). As
mentioned above, since the material was solution treated and
3. Results water quenched, the microstructure consisted of uniformly-dis-
tributed acicular martensite. It should be noted that the CM spe-
3.1. Vickers hardness and microstructures cimen exhibits ner and more uniformly-distributed martensite
than the SLM-quenched one.
Vickers hardness of three types of specimens, that is, SLM, SLM- In the SLM and SLM-quenched specimens, many microscopic
quenched and CM, was obtained as an average for 20 points defects (size o50 mm) are seen. The examples of such defects are
measurement. Vickers hardness is shown in Fig. 2. The average shown in Fig. 4(a) and (b), that is, cylindrical and angular defects,
M. Akita et al. / Materials Science & Engineering A 666 (2016) 1926 21

10
m 10
0m

10
m 10
0m

10
m 10m

Fig. 3. Microstructures: (a) 3D macroscopic appearance of SLM specimen, (b), (c) SLM specimen, (d), (e) SLM-quenched specimen, (f), (g) CM specimen. Arrows indicate
ferrite-rich area.
22 M. Akita et al. / Materials Science & Engineering A 666 (2016) 1926

1 0m 10m

Fig. 4. Micrographs showing the defects in SLM specimen.

respectively. It is considered that the powder of type 630 did not were 400 MPa, 500 MPa and 700 MPa for the SLM, SLM-quenched
melt properly during the SLM process, resulting in porosities and CM specimens, respectively. Fig. 7 shows crack length, 2c, as a
whose sizes are comparable to the laser-lamination thickness, function of the number of cycles, N, (Fig. 7a) and the cycle ratio, N/
50 mm (See Section 2.1). Several studies described that some un- Nf (Fig. 7b), where Nf is the number of cycles to failure. In the SLM
melted-powder regions were observed due to inadequate energy specimen, owing to the limitation of specimen number, the run-
input [2729]. This suggests that the crack initiation resistances of out specimen (sw 300 MPa, N 107 cycles) was used for crack
the SLM and SLM-quenched specimens might be lower than that growth test. Therefore, SLM specimen exhibits load history.
of the CM one. However, it should be noted that load history before fatigue crack
initiation hardly affects fatigue crack growth behavior, because
3.2. Fatigue strength fatigue crack growth is dominated by severe plastic deformation at
the crack tips. The tendency of fatigue crack growth behavior is not
Fig. 5 shows S-N diagram of three materials. The fatigue clear in Fig. 7(a). But when crack initiation life is estimated using
strengths of the SLM and SLM-quenched specimens were much N/Nf (Fig. 7b), it is clear that crack initiation lives of the SLM and
lower than those of the CM one. The fatigue limits of the SLM, SLM-quenched specimens are much shorter than that of the CM
SLM-quenched and CM specimens at 107 cycles were 350 MPa, one, indicating the lower crack initiation resistances in the SLM
400 MPa and 550 MPa, respectively. The fatigue strength of SLM- and SLM-quenched specimens. The SLM specimen suddenly failed
quenched specimen was slightly higher than the SLM one, but was with the crack length shorter than 1 mm. That is because multiple
still lower than the CM one. cracks initiations and coalescence occurred.
Subsequently, to evaluate crack growth resistances, the re-
3.3. Fatigue crack initiation and early crack growth lationships between crack growth rate, da/dN, and maximum
stress intensity factor, Kmax, are revealed in Fig. 8, where the stress
Fig. 6 reveals typical fracture surfaces near crack initiation sites intensity factor was calculated using an analytical solution by
of three types of specimens. In the SLM (Fig. 6(a) and (b)) and Shiratori et al. [30], assuming an aspect ratio, a/c1 (a: crack
SLM-quenched (Fig. 6(c) and (d)) specimens, defects, which sizes depth, c: half crack length on surface). In the SLM specimen, the
approximately 70100 mm, were seen at the fatigue crack initiation crack growth rates gradually increased. In the SLM-quenched
sites. In the CM specimen (Fig. 6e), fatigue crack initiated at the specimen, the crack growth rates rapidly decreased around
specimen surface due to cyclic slip deformation, showing at crack Kmax 6 MPam1/2, and then increased. The da/dN - Kmax relation-
initiation site. ships of the SLM and SLM-quenched specimens are similar around
The early crack growth behavior was monitored by a plastic Kmax 510 MPam1/2. On the other hand, the crack growth rates of
replication technique. The stress amplitude, sa, of the crack growth the CM specimen were higher than those of the SLM and SLM-
test was determined as the value at which the fatigue life would be quenched ones at the medium Kmax range. At the Kmax level larger
approximately 105 cycles. Thus, the stress amplitudes employed than 30 MPam1/2, the da/dN - Kmax relationship of the CM speci-
men merged into that of the SLM-quenched one. It could be
concluded that the crack growth resistances of the SLM and SLM-
10
000
Type 630 SLM
M quenched specimens were higher than that of the CM one.
Stress amplitude a (MPa)

9
900 Mquenched
SLM
CM
8
800
4. Discussion
7
700
4.1. Effect of SLM on fatigue strength
6
600
5
500 As shown in Fig. 5, the fatigue strengths of the SLM and SLM-
quenched specimens were much lower than those of the CM one.
4
400
Generally, the fatigue strength in steels depends on their hardness.
Rotary bending
3
300 Vickers hardness of the SLM (275 HV) and SLM-quenched speci-
Laboratory air
men (340 HV) was lower than that of the CM one (454 HV). In
200 4
2 5 6 7 8 addition, it is known that the fatigue limit, sw, linearly increases
10 10 10 10
0 10
with increasing Vickers hardness in the range of 100 oHV o 400.
Number of cycles to failure N f
The linear relation is given as follows; sw 1.6 HV [31,32]. This
Fig. 5. S-N diagram. equation is widely used for mechanical design, because the fatigue
M. Akita et al. / Materials Science & Engineering A 666 (2016) 1926 23

50m 10m

300m 30m

50m
Fig. 6. SEM micrographs showing fracture surfaces near crack initiation sites: (a) SLM specimen (sa 450 MPa, Nf 4.0  104), (b) magnied view of (a), (c) SLM-quenched
specimen (sa 350 MPa, Nf 1.0  107), (d) magnied view of (c), (e) CM specimen (sa 650 MPa, Nf 3.3  105). Arrows indicate defects.

4 4
Surface crack length 2 c (mm)

Type 630
Surface crack length 2 c (mm)

Type 630
Rotary bending Rotary bending
Laboratory air Laboratory air
3 3 SLM ( a =400MPa)
SLM SLMquenched ( a =500MPa)
(a=400MPa) CM ( a =700MPa)
2 SLMquenched
( a= 500MPa) 2
CM ( a = 700MPa)

1 1

0 2 3 4 5 6 7 0
10 10 10 10 10 10 0 0.2 0.4 0.6 0.8 1
Number of cycles N Cycle ratio N/N f
Fig. 7. Surface crack length 2c as a function of (a) number of cycles, N, (b) cycle ratio, N/Nf.

limit could be roughly estimated using a hardness value. Fig. 9 lower limit of scatter band. This means that the fatigue limits of
indicates the relationship between sw and HV, where the scatter the SLM and SLM-quenched specimens are low in terms of their
band of several steels is indicated by the dotted line [32]. The data hardness. The reason of this behavior is as follows; as mentioned
points of the SLM and SLM-quenched specimens are out of the in Section 3.3, fatigue cracks in the SLM and SLM-quenched
24 M. Akita et al. / Materials Science & Engineering A 666 (2016) 1926

Type 630

Loading direction
3
Rotary bending
10 Laboratory air
Crack growth rate da/dN (mm/cycle)

Defect

4
10
Branching
5
10
30m

6 Fig. 10. An example of optical micrograph showing crack initiation site in the SLM
10 specimen.
SLM
(a=400MPa)
7 SLMquenched 4.2. Fatigue crack initiation and early-stage growth
10 (a=500MPa)
CM
(a =700MPa) Fatigue cracks initiated from defects near the surfaces in the
8 SLM and SLM-quenched specimens (See Section 3.3). For example,
10
as shown in Fig. 7, the crack initiation of the SLM-quenched spe-
1 2 5 7 10 20 50 70100 cimen was signicantly earlier than the CM one. Defects could
Maximum stress intensity factor enhance early crack initiation. Fig. 10 reveals the small crack just
1/2 after the initiation in the SLM specimen. It should be noted that
Kmax (MPam )
the crack initiated from the defect is indicated by an arrow. Fig. 11
Fig. 8. Relationship between crack growth rate, da/dN, and maximum stress in- shows the SLM-quenched specimen surface observed during crack
tensity factor, Kmax. growth test. Before crack growth test, small defects (o5 mm) were
detected in line (Fig. 11a). Crack initiation occurred at that linearly-
aligned defects and crack propagated along the line in the early
700 stage of crack growth test (Fig. 11b). The crack length estimated on
Type 630 the specimen surface from Fig. 11(b) is about 150 mm, and that
SLM crack length was used for the calculation of Kmax in Fig. 8. But the
600
w (MPa)

SLMquenched small crack coalescence occurred along the linearly-aligned de-


CM fects. It implies that the crack length in the depth direction would
be shorter than the length on the specimen surface (150 mm).
500 Therefore, the drop of crack growth rates of the SLM-quenched
specimen in the early stage (Fig. 8) could be attributed to the
400 overestimation of Kmax value calculated assuming an aspect ratio,
Fatigue limit

a/c1.
Fig. 12 shows the optical micrographs indicating crack growth
300 paths observed on plastic replicas. The crack deection and
branching were observed in the SLM and SLM-quenched speci-
mens (Fig. 12(a) and (b)). Frequent deection and branching in the
200 w=1.6HV crack growth paths could decrease the crack growth rate at a given
Scatter band Kmax (see Fig. 8) in the SLM and SLM-quenched specimens. On the
other hand, the crack in the CM specimen grew straight manner
100 after initiation (Fig. 12c). It could be concluded that the fatigue
0 100 200 300 400 500
crack growth resistances in both SLM specimens were enhanced
Vickers hardness HV by the deection and branching of crack path. The frequent crack
Fig. 9. Fatigue limit as a function of Vickers hardness. deection and branching are attributed to the microstructural
inhomogeneity and defects in the SLM specimens.

specimens initiated from defects near surface (Fig. 6(ad)). Gong 4.3. da/dN-K/E relationships
et al. indicated that the defects brought on the decrease of fatigue
strength in the SLMed Ti-6Al-4V alloy [33]. Defects are generated The crack growth behavior of the SLM, SLM-quenched and CM
due to incomplete powder melting or improper fusion at the specimens was shown in Fig. 8. The results should be compared
successive tracks or layers during the SLM process. It is considered with those in the other metallic materials. It is well known that
the fatigue crack growth behavior can be related to the elastic
that the lower hardness and defects have detrimental effects on
modulus, E. Fig. 13 summarizes the fatigue crack growth re-
the fatigue strengths in both SLM specimens. On the other hand,
sistances characterized in terms of K/E. It is also known that
the fatigue limit of CM specimen is also lower than the expected
fatigue crack growth resistances in many metallic alloys, that is,
value from the hardness. The Vickers hardness of CM specimen is mild steels, wrought Al alloys, cast Al alloy, cupper, Ti alloys and Zr
454 HV, and exceeds the limitation value of 400 HV, in which alloy, are within the band enclosed by dotted line [34]. Since these
sw 1.6 HV is empirically valid. Therefore, it is considered that the results were obtained at a stress ratio, R, of 0, K is equivalent to
equation, sw 1.6 HV, is not held in the range of HV 4400, re- the Kmax under R 1 in the present study. In the data plotted on
sulting in an overestimation of fatigue limit in the CM specimen da/dN-K/E relationship, where E 174 GPa in Table 1 was used,
from its hardness. the results of SLM and SLM-quenched specimens are within the
M. Akita et al. / Materials Science & Engineering A 666 (2016) 1926 25

Loading direction

30m 30m

Fig. 11. Optical micrographs showing crack initiation in the SLM-quenched specimen: (a) before crack growth test, N 0 cycle. (b) N 1.0  103 cycles, N/Nf 0.2.

Crack initiation

50m

Branching:
Branching: Crack initiation 100m
Loading direction

Crack initiation

100m

Fig. 12. Macroscopic appearances of crack growth paths: (a) SLM specimen (sa 400 MPa, N 1.7  104 cycles), (b) SLM-quenched specimen (sa 500 MPa, N 4.4  105
cycles), (c) CM specimen (sa 700 MPa, N 8.0  104 cycles).

2 specimens are similar to the other metallic materials, while the


10 Type 630 CM specimen has slightly lower growth resistance. In the present
Rotary bending study, the SLM and SLM-quenched specimens had lower fatigue
3 Laboratory air strengths than the CM one in spite of higher growth resistances.
Crack growth rate da/dN (mm/cycle)

10 That is because specimen size is relatively small as shown in Fig. 1,


and consequently fatigue lives are mainly dominated by fatigue
4
crack initiation resistances.
10
R=0
5. Conclusion
5
10
Fatigue tests of type 630 stainless steel fabricated by selective
laser melting (SLM) method were conducted. Post-heat-treated
6 (SLM-quenched) and conventionally-melted (CM) type 630 were
10
also used for comparison. The fatigue strengths and crack growth
SLM behavior were discussed on the basis of the results of fatigue tests
(a=400MPa)
7 and fractographic observations. The results obtained are as
10 SLMquenched
follows.
(a=500MPa)
CM
8 (a =700MPa) 1) In the CM specimen, the microstructure consisted of uniformly-
10 distributed ne acicular martensite. In the SLM specimen, fer-
1 2 5 10 20 50 rite-rich areas were recognized due to the slow cooling rate
5 during SLM process. Quenching after SLM process could make
( 10 )
1/2 the macrostructure uniformly-distributed ne acicular marten-
K / E m
site, while the acicular martensite was still coarser than the CM
Fig. 13. Crack growth rate, da/ dN, as a function of K/E. specimen. In addition, small defects (o50 mm) were seen in the
SLM and SLM-quenched specimens, which were formed during
band. On the other hand, the data of CM specimen are on the additive lamination of melted powder.
upper boundary of the band. Therefore, it is concluded that the 2) Depending on the microstructure, the hardness of SLM (275 HV)
fatigue crack growth resistances of SLM and SLM-quenched and SLM-quenched (340 HV) specimens was lower than the CM
26 M. Akita et al. / Materials Science & Engineering A 666 (2016) 1926

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